TY - CONF A1 - Kotthoff, Lisa A1 - Koch, Matthias A1 - Schwerdtle, T. T1 - Kopplung von Elektrochemie mit LC/MS zur Simulation von Transformationsprodukten - Untersuchung von Monensin N2 - Die Identifizierung von Transformationsprodukten (TPs) von Tierarzneimittelwirkstoffen ist wichtig für Gesundheit, Lebensmittel und Umwelt. Monensin (MON) gehört zu den Ionophoren Antibiotika und wird genutzt zum Schutz und zur Behandlung von Kokzidiose bei Geflügel, vorwiegend prophylaktisch in der Geflügelmast. Rückstände können in tierischen Produkten (Geflügel und Eier) aber auch in der Umwelt (Tiermist, Gewässer, Böden) gefunden werden. Verschiedene Transformationsprozesse können auftreten, beginnend bei der Biotransformation in lebenden Organismen bis hin zu biotischen und abiotischen Prozessen in der Umwelt. Die Kopplung von Elektrochemie und Massenspektrometrie, kurz EC/HRMS, als rein instrumenteller Ansatz zur Simulation von Transformationsprodukten ist seit vielen Jahren in der pharmazeutischen Forschung etabliert. Hierbei wird mithilfe einer elektrochemischen Durchflusszelle der oxidative Metabolismus einer Substanz simuliert und zugleich analysiert. Unter Verwendung von EC/HRMS und LC-HRMS wurde MON elektrochemisch bei Potentialen bis zu 2.5 V vs Pd/H2 oxidiert und die entstehenden TPs mit Metabolismustests mit Rattenlebermikrosomen verglichen. Als Ergebnis wurden verschiedene TPs von MON gefunden und Strukturvorschläge wurden erstellt. Ein Überblick über die detektierten und identifizierten TPs wird dargestellt. T2 - Lebensmittelsicherheit in Deutschland - was bleibt? CY - Potsdam-Rehbrücke, Germany DA - 04.06.2019 KW - Transformationsprodukte KW - Elektrochemie KW - Ionophore Antibiotika KW - Hochauflösende Massenspektrometrie PY - 2019 AN - OPUS4-48155 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material studies of the Dead Sea Scrolls N2 - Our study is dedicated to non-destructive characterization of the support and the inks of the DSS. To that aim we use micro-XRF, 3D- SY-XRF, different IR methods including synchrotron radiation based reflectance spectroscopy, optical and electron microscopy. The lecture discusses advantages and the shortcomings of the non-destructive testing approach. T2 - Seminar CY - Freie Universität Berlin, Germany DA - 04.02.2019 KW - Dead Sea Scrolls PY - 2019 AN - OPUS4-48132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Rashid, R. A1 - Munir, R. A1 - Zaidi, N. T1 - Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia N2 - Background: Cancer cells modify the balance between fatty acid (FA) synthesis and uptake under metabolic stress, induced by oxygen/nutrient deprivation. These modifications were shown to alter the levels of individual triglyceride (TG) or phospholipid sub-species. To attain a holistic overview of the lipidomic profiles of cancer cells under stress we performed a broad lipidomic assay, comprising 244 lipids from six major classes. This assay allowed us to perform robust analyses and assess the changes in averages of broader lipid-classes, stratified on the basis of saturation index of their fatty-acyl side chains. Methods: Global lipidomic profiling using Liquid Chromatography-Mass Spectrometry was performed to assess lipidomic profiles of biologically diverse cancer cell lines cultivated under metabolically stressed conditions. Results: Neutral lipid compositions were markedly modified under serum-deprived conditions and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains. In contrast and unexpectedly, no robust changes were observed in lipidomic profiles of hypoxic (2% O2) Cancer cells despite concurrent changes in proliferation rates and metabolic gene expression. Conclusions: Serum-deprivation significantly affects lipidomic profiles of cancer cells. Although, the levels of individual lipid moieties alter under hypoxia (2% O2), the robust averages of broader lipid classes remain unchanged. KW - Tumor metabolism KW - Fatty acid metabolism KW - Lipidomic profile KW - Metabolic stress PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481061 DO - https://doi.org/10.1186/s12885-019-5733-y SN - 1471-2407 VL - 19 SP - 501, 1 EP - 11 PB - Springer Nature AN - OPUS4-48106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Materialwissenschaftliche Untersuchungen an Qumranrollen N2 - Heute stimmen die meisten Gelehrten und Historiker darin überein, dass die Höhlen von Qumran eine Essener-Bibliothek beherberg-ten. Über ihren Ursprung, sowie die Herkunft der einzelnen Schriften, wird noch immer rege debattiert. Der aktuelle Beitrag präsentiert detaillierte Lösungsansätze zu Klärung der Provenienzfrage der Schriftrollen von Qumran. T2 - Vorlesungsreihe CY - Freie Universität Berlin, Germany DA - 14.01.2019 KW - Qumranrollen PY - 2019 AN - OPUS4-48133 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira A1 - Hahn, Oliver T1 - Material analysis of manuscripts: methodological introduction N2 - Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question and the choice of the methods to obtain the requested answer. Therefore, one should try to go beyond the understanding of the basic principles of the scientific analysis. We will start with a glance at the basic principles of the techniques used in the material science for determination of the elemental composition (X-ray emission) and molecular composition (FTIR & Raman). We will move then to the bench and mobile equipment commonly used in the field of cultural heritage. At the end we will choose a question to be answered and design an ideal experiment that will be modified according to the limitations dictated by on-site conditions. In the ateliers in the afternoon we will a) compare two XRF devices that differ in their spatial resolution; b) use a high resolution microscope (Keyence) to obtain a close look at writing surfaces and materials; c) we will learn to determine the type of the inks with the help of another microscope (DinoLite AD413T-12V), a usb microscope with visible, UV and NIR illumination; d) we will learn to use FTIR-ATR device for determination of the type of the writing surface; e) We will use mobile Raman device for identification of pigments. T2 - Summer School: Manusciences19 CY - Frejus, France DA - 10.03.2019 KW - Material science KW - Cultural heritage PY - 2019 AN - OPUS4-48137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Detection of microplastics using thermoanalytical methods  N2 - The presentation summarized the use of thermal analytic methods for the detection of microplastics. T2 - Workshop State of teh art of anylatical methodes for reliable detection of micro- and nanoplastics CY - Ispra, Italy DA - 13.05.2019 KW - microplastics, sampling, sampling techniques, water PY - 2019 AN - OPUS4-48119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Lehnik-Habrink, Petra A1 - Bandow, Nicole A1 - Sauer, Andreas T1 - Validation of European horizontal methods for the analysis of PAH, PCB and dioxins in sludge, treated biowaste and soil N2 - Draft standards for the determination of organic pollutants in the solid matter of environmental matrices such as sludge, treated biowaste and soil have been basically developed in the framework of the European standardization project HORIZONTAL. A research project financed by the German Federal Environment Agency was initiated to finalize some of these CEN standard drafts, since fully validated standard procedures are crucial for the evaluation of their reliability in the context of implementation in legislation on environmental health. Approach: Appropriate test materials (< 2mm particle size) were prepared and homogenized from contaminated soils, sludge and treated biowaste containing polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), dioxins, furans and dioxin-like-PCB and served, along with reference solutions, as the basis for international interlaboratory comparisons. Performance data of three analytical standard procedures were obtained by the statistical evaluation of results received from 11 to 29 participants per test material. Results: The overall variation coefficients of reproducibility (between-lab standard deviations) for the sum parameters were roughly between 10 and 35 %. The variation coefficients of repeatability (within-lab standard deviations) range between 3 % and 8 % and show no trend considering the substance groups or matrices. The highest coefficients of reproducibility were found for the analysis of PAHs, which were between 26 and 35 %, depending on the matrix, whereas 7-17 % reproducibility was observed for toxicity equivalents (TEQ) comprising dioxins, furans and dl-PCB. Conclusions: Overall, the results confirm that the procedures described in the Technical Specifications are fit for purpose for all three matrices and that the feasibility of the HORIZONTAL approach, to cover several matrices with one standard per analyte, was thereby proven. KW - Standardization KW - Analytical methods KW - Organic contaminants KW - Validation trial KW - Interlaboratory comparison PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479914 DO - https://doi.org/10.1186/s12302-019-0211-3 SN - 2190-4715 VL - 31 SP - 29, 1 EP - 10 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Fink, Friedrich A1 - Noll, M. T1 - Hybridmodell zur Bestimmung des Ligningehalts von Kiefernholz N2 - Die Untersuchungen sind durch das das DFG Schwerpunktprogramm 1374 für Biodiversitätsforschung motiviert. Anhand des überwachten Abbaus von Totholz soll untersucht werden, welche Auswirkung unterschiedliche Formen und Intensitäten der Landnutzung auf die Biodiversität innerhalb von drei Exploratorien zeigen. Bei den vorangegangenen Studien wurden Nahrungs¬netzte auf organismischer Ebene sowie Klima- und Umgebungsdaten untersucht und die Veränderung des ausgebrachten Totholzes als Masseverlust erfasst. Es wird jedoch erwartet, dass in Anhängigkeit der beteiligten Organismen und Umgebungsparameter verschiedene Mechanismen des Holzabbaus vorliegen, die in unterschiedlichen Abbauraten der Holzkomponenten Lignin, Cellulose und Hemicellulose resultieren. Aus diesem Grund ist die quantitative Untersuchung des Ligningehalts an Hölzern ein wesentlicher Schritt für ein verbessertes Verständnis der Biodiversität in den untersuchten Exploratorien. Um der hohen Probenanzahl, die sich aus der Kontrolle von jeweils 100 Proben (Plots) in den drei Exploratorien für Hölzer aus 13 Baumarten ergibt, gerecht zu werden, wird eine schnelle und effiziente Untersuchungsmethode benötigt. Diese wird derzeit in Form einer NIR-spektroskopischen Bestimmung des Ligningehalts entwickelt. Um basierend auf den NIR Spektren vermahlener Holzproben Lignin und weitere Holzkomponenten korrekt vorherzusagen, muss zunächst basierend auf nasschemischen Analysen ein chemometrisches Modell kalibriert werden. Dazu ist die Charakterisierung von mindestens 20 – 30 Proben, die eine hohe Varianz des Ligningehalts aufweisen, notwendig. Im Vortrag werden erste Untersuchungs¬ergebnisse für die Vorhersage des Ligningehalts von Kiefernhölzern, die für ein Jahr in dem Exploratorium Schorfheide exponiert wurden, vorgestellt. Die anschließende explorative Datenanalyse (PCA) unter Verwendung von insgesamt 28 Variablen zur Beschreibung klimatischer und Umgebungsparameter weist eine Reihe interessanter Korrelationen auf. Demnach ist der Ligningehalt auf der ersten Hauptkomponente (29% erklärte Varianz) positiv mit dem C/N-Verhältnis und negativ mit Landnutzungsindex korreliert. Masseverlust und Temperatur hingegen dominieren die zweite Hauptkomponente (12% erklärte Varianz). T2 - 4. Innovationsakademie Lignocellulose CY - Berlin, Germany DA - 11.04.2019 KW - NIR Spektroskopie KW - Lignin KW - Datenanalyse PY - 2019 AN - OPUS4-47963 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dümichen, Erik A1 - Eisentraut, Paul A1 - Celina, M. A1 - Braun, Ulrike T1 - Automated thermal extraction-desorption gas chromatography mass spectrometry: A multifunctional tool for comprehensive characterization of polymers and their degradation products N2 - The TED-GC-MS analysis is a two-step method. A sample is first decomposed in a thermogravimetric analyzer (TGA) and the gaseous decomposition products are then trapped on a solid-phase adsorber. Subsequently, the solid-phase adsorber is analyzed with thermal desorption gas chromatography mass spectrometry (TDU-GC-MS). This method is ideally suited for the analysis of polymers and their degradation processes. Here, a new entirely automated System is introduced which enables high sample throughput and reproducible automated fractioned collection of decomposition products. Strengths and limitations of the system configuration are elaborated via three examples focused on practical challenges in materials analysis and identification: i) separate analysis of the components of a wood-plastic-composite material, ii) quantitative determination of weight concentration of the constituents of a polymer blend and iii) quantitative analysis of model samples of microplastics in suspended particulate matter. KW - Thermal extraction-desorption gas chromatography mass spectrometry KW - Analysis KW - Polymers KW - Microplastics KW - Automation PY - 2019 DO - https://doi.org/10.1016/j.chroma.2019.01.033 VL - 1592 SP - 133 EP - 142 PB - Elsevier CY - Amsterdam AN - OPUS4-48287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotthoff, Lisa A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - Electrochemistry coupled to LC/HRMS to investigate transformation products of the veterinary drug monensin N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for health, food and environmental matters. Monensin (MON) is an ionophore antibiotic widely used to cure and prevent coccidiosis by chicken especially in broiler farming. Residues can be found in food products (chicken and eggs) and in the environment (manure, soil, water). Several transformation processes can alter the parent compound MON, ranging from biotransformation in living organism to biotic/abiotic and microbial processes in environmental matters. The main objective of this work was to investigate the potential of electrochemistry (EC) to simulate oxidative transformation processes of MON and to predict TPs. An electrochemical reactor was used consisting of a flow-through cell with a glassy carbon working electrode. Derived TPs were analyzed by online coupling of EC and high-resolution mass spectrometry (HRMS) and LC/HRMS offline measurements. Among the generated TPs already known as well as unknown TPs of MON could be found. Additionally, MON was subjected also to other transformation experiments like metabolism tests with rat microsomes or the pH-dependent hydrolysis. As a result, different targeted and suspected TPs could be identified by analysis with LC/HRMS. An overview of detected/identified TPs from this study will be presented in comparison to literature known metabolites and TPs. T2 - ElCheMS 2019 – 5th Workshop on Electrochemistry/Mass Spectrometry 2019 CY - Münster, Germany DA - 11.06.2019 KW - Transformation product KW - Electrochemistry KW - High-resolution MS KW - Ionophore antibiotic PY - 2019 AN - OPUS4-48209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geilert, Sonja A1 - Vogl, Jochen A1 - Rosner, M. A1 - Eichert, T. T1 - Boron isotope variability related to boron speciation (change during uptake and transport) in bell pepper plants and SI traceable n(11B)/n(10B) ratios for plant reference materials N2 - Rationale: Boron (B) is an essential micronutrient in plants and its isotope variations are used to gain insights into plant metabolism, which is important for crop plant cultivation. B isotope variations were used to trace intra‐plant fractionation mechanisms in response to the B concentration in the irrigation water spanning the range from B depletion to toxic levels. Methods: A fully validated analytical procedure based on multi‐collector inductively coupled plasma mass spectrometry (MC‐ICP‐MS), sample decomposition and B Matrix separation was applied to study B isotope fractionation. The Validation was accomplished by establishing a complete uncertainty budget and by applying reference materials, yielding expanded measurement uncertainties of 0.8‰ for pure boric acid solutions and ≤1.5‰ for processed samples. With this validated procedure SI traceable B isotope amount ratios were determined in plant reference materials for the first time. Results: The B isotope compositions of Irrigation water and bell pepper samples suggest passive diffusion of the heavy 11B isotope into the roots during low to high B concentrations while uptake of the light 10B isotope was promoted during B depletion, probably by active processes. A systematic enrichment of the heavy 11B isotope in higher located plant parts was observed (average Δ11Bleaf‐roots = 20.3 ± 2.8‰ (1 SD)), possibly by a facilitated transport of the heavy 11B isotope to growing Meristems by B transporters. Conclusions: The B isotopes can be used to identify plant metabolism in Response to the B concentration in the irrigation water and during intra‐plant B transfer. The large B isotope fractionation within the plants demonstrates the importance of biological B cycling for the global B cycle. KW - isotope fractionation KW - boron KW - delta value KW - metabolism KW - bell pepper KW - SI traceability KW - measurement uncertainty PY - 2019 DO - https://doi.org/10.1002/rcm.8455 SN - 1097-0231 SN - 0951-4198 VL - 33 IS - 13 SP - 1137 EP - 1147 PB - John Wiley & Sons Ltd. AN - OPUS4-48213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred A1 - Seneschal-Merz, Karine A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Determination of boron in 19th and 20th century paint layers using LIBS N2 - 19th and 20th centuries glass paint layers consist of a colour body and a colourless lead silicate flux, in which borax or boric acid was added as further component to improve the paint ability and to reduce the firing temperature for multiple layers of paint. Model glasses were used in laboratory tests to investigate the stability of glass paints with additions of boron oxide. To determine boron in paint layers, a LIBS-system with pulsed NdYAG-laser was used. T2 - Technart 2019 CY - Brugge, Belgien DA - 07.05.2019 KW - Stained glass windows KW - Glass paints KW - LIBS PY - 2019 AN - OPUS4-48229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul A1 - Goedecke, Caroline A1 - Dümichen, E. A1 - Braun, Ulrike T1 - Detektion von Mikroplastik mittels Thermoextraktion Desorption Gas Chromatographie Massen Spektrometrie (TED-GC-MS) N2 - Das Poster gibt eine kurze Einleitung in die Thematik Mikroplastik in der Umwelt. Das Funktionsprinzip des Verfahrens und einige Kenndaten werden dargestellt. Optimierte Verfahrensparameter werden aufgezählt und Teilergebnisse aus zwei Messkampagnen gezeigt. T2 - Abschlusskonferenz BMBF-Projekt MiWa CY - Karlsruhe, Germany DA - 09.09.2019 KW - Mikroplastik KW - TED-GC-MS KW - Optimierung PY - 2019 AN - OPUS4-49117 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Borzekowski, Antje A1 - Anggriawan, R. A1 - Auliyati, M. A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. A1 - Karlovsky, P. A1 - Maul, Ronald T1 - Formation of Zearalenone Metabolites in Tempeh Fermentation N2 - Tempeh is a common food in Indonesia, produced by fungal fermentation of soybeans using Rhizopus sp., as well as Aspergillus oryzae, for inoculation. Analogously, for economic reasons, mixtures of maize and soybeans are used for the production of so-called tempeh-like products. For maize, a contamination with the mycoestrogen zearalenone (ZEN) has been frequently reported. ZEN is a mycotoxin which is known to be metabolized by Rhizopus and Aspergillus species. Consequently, this study focused on the ZEN transformation during tempeh fermentation. Five fungal strains of the genera Rhizopus and Aspergillus, isolated from fresh Indonesian tempeh and authentic Indonesian inocula, were utilized for tempeh manufacturing from a maize/soybean mixture (30:70) at laboratory-scale. Furthermore, comparable tempeh-like products obtained from Indonesian markets were analyzed. Results from the HPLC-MS/MS analyses show that ZEN is intensely transformed into its metabolites alpha-zearalenol (alpha-ZEL), ZEN-14-sulfate, alpha-ZEL-sulfate, ZEN-14-glucoside, and ZEN-16-glucoside in tempeh production. alpha-ZEL, being significantly more toxic than ZEN, was the main metabolite in most of the Rhizopus incubations, while in Aspergillus oryzae fermentations ZEN-14-sulfate was predominantly formed. Additionally, two of the 14 authentic samples were contaminated with ZEN, alpha-ZEL and ZEN-14-sulfate, and in two further samples, ZEN and alpha-ZEL, were determined. Consequently, tempeh fermentation of ZEN-contaminated maize/soybean mixture may lead to toxification of the food item by formation of the reductive ZEN metabolite, alpha-ZEL, under model as well as authentic conditions. KW - Modified mycotoxins KW - Zearalenone sulfate KW - a-zearalenol KW - Food fermentation KW - Rhizopus and Aspergillus oryzae PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491126 DO - https://doi.org/10.3390/molecules24152697 VL - 24 IS - 15 SP - 2697 PB - MDPI AN - OPUS4-49112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul A1 - Dümichen, E. A1 - Goedecke, Caroline A1 - Braun, Ulrike T1 - Mikroplastik-Bestimmung mit TED-GC-MS N2 - Der Vortrag beschreibt den Entwicklungsprozess des Analysenverfahrens TED-GC-MS zur Bestimmung von Mikroplastikgehalten in Umweltproben im Rahmen des BMBF-Projektes MiWa. Die Funktionsweise, die Automatisierung und die Optimierung einzelner Geräteparameter und Leistungsdaten werden gezeigt. Untersuchungen des Einflusses von Probenmatrices werden dargestellt und die Ergebnisse einiger Messkampagnen und Ringversuche vorgestellt, die die Routinefähigkeit des Verfahrens dokumentieren. T2 - MiWa-Abschlusskonferenz CY - Karlsruhe, Germany DA - 10.09.2019 KW - Mikroplastik KW - Thermoanalyse KW - TED-GC-MS PY - 2019 AN - OPUS4-49115 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - ZRM für die Nichtmetall-Analytik N2 - Die Vorgehensweise bei der Zertifizierung von Referenzmaterialien in der BAM entsprechend den Regeln des ISO-Guide 35 wird an Beispielen beschrieben. Darüber hinaus wird ein umfassender Überblick über Referenzmaterialien zur Analyse der Nichtmetalle Sauerstoff, Wasserstoff, Stickstoff, Kohle und Schwefel gegeben. T2 - Expertentreffen anorganische Materialanalyse CY - Langenselbold, Germany DA - 11.09.2019 KW - ZRM KW - Nichtmetall-Analytik KW - ISO-Guide 35 KW - Referenzmaterialien PY - 2019 AN - OPUS4-49091 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Wander, Lukas A1 - Bremser, Wolfram A1 - Kipphardt, Heinrich T1 - NIR-Ringversuch II: Erste Ergebnisse N2 - Vorstellung der Ergebnisse des Ringversuchs NIR II für den Analyten Paracetamol. Neben den "S-Shape" Darstellungen für die Levels A, B und C werden En-Werte und eine Darstellung der relativen Unsicherheiten (Horwitz) gezeigt. Alle beteiligten Labors zeichnen sich durch eine hohe Performance aus. T2 - 15. Ttreffen PAT RFA CY - Lonza, Visp, Switzerland DA - 17.09.2019 KW - Nahinfrarotspektroskopie KW - Ringversuch PY - 2019 AN - OPUS4-49043 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Ein Blick in die Welt der Mechanochemie N2 - Perhaps due in no small part to its historical mystique, mechanochemistry has been shrowded in relative obscurity for quite some time. The successes of mechanochemistry in organic synthesis have often been curtailed by a fundamentally limited mechanistic understanding. Lately, however, the community has made great strides towards understanding the fundamentals, as well as large steps forward regarding industrially significant scale-up via twin-screw extrusion. A variety of recent work has traded in some of mechanochemistry’s mystique for simple, straight-forward chemical guidelines. T2 - Seminar Anorganische Chemie Universität Kiel CY - Kiel, Germany DA - 22.10.19 KW - Mechanochemistry KW - XRD PY - 2019 AN - OPUS4-50134 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Shaken or levitated? A time resolved perspective on unconventional crystallization N2 - This Outlook provides a brief overview of the recent achievements and opportunities created by acoustic levitation and mechanochemistry, including access to materials, molecular targets, and synthetic strategies that are difficult to access by conventional means. T2 - Vortragsreihe Analytik Merck CY - Darmstadt, Germany DA - 18.11.19 KW - Levitation KW - Acoustic levitation KW - X-ray and electron diffraction PY - 2019 AN - OPUS4-50135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Harmonization in microplastics Analysis N2 - The lecture summarizes the current status of hamonization edr microplastics analytics in Germany. T2 - Symposium on Occurrence and Fate of Microplastics CY - Beijing, China DA - 09.07.2019 KW - Microplastics KW - TED-GC-MS KW - Harmonisation PY - 2019 AN - OPUS4-49063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Eisentraut, Paul A1 - Kalbe, Ute A1 - Wachtendorf, Volker T1 - Elastomere und TPE – Gut für die Umwelt? – Kreislaufwirtschaft und Normung vereinen N2 - Der Vortrag fasst Projekte an der BAM mit Hinblick auf Elastomere und Umweltthemen zusammen. T2 - DIN Workshop: Elastomere und TPE – Gut für die Umwelt? – Kreislaufwirtschaft und Normung vereinen CY - Berlin, Germany DA - 08.08.2019 KW - Mikroplastik KW - Reifenabrieb KW - Sportböden PY - 2019 AN - OPUS4-49064 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Messen ist nicht alles, aber ohne Messmethoden ist alles nichts!  N2 - Der Vortrag fasst den aktuellen Methodenstand bei der Analytik für Mikroplastik zusammen. T2 - FACHFORM „Mikroplastik“ anlässlich VUP-Jahrestagung 2019 CY - Gießen, Germany DA - 05.09.2019 KW - Mikroplastik KW - TED-GC-MS KW - Hamonisierung PY - 2019 AN - OPUS4-49066 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Bannick, C.G. T1 - Analytik von Mikroplastik - Verfahren-Ergebnisse-Harmonisierung N2 - Die zunehmenden Nachweise von Kunststoffen in verschiedenen Umweltmedien erfahren in den letzten Jahren weltweit ein zunehmendes wissenschaftliches, gesellschaftliches und politisches Interesse. Besondere Aufmerksamkeit erfahren Kunststoffpartikel von 1-1.000 µm, sogenanntes Mikroplastik. Es wurde mittlerweile in Wasser, Böden, Luft und Biota nachgewiesen. Obwohl die Wirkungen auf die natürlichen Umweltfunktionen noch unklar sind und kontrovers diskutiert werden, ist allein durch die ubiquitäre Präsenz eine systematische Erfassung von Eintragsquellen und Verbleib der Partikel über alle Umweltmedien notwendig, um Maßnahmen zur Reduktion der Einträge zu veranlassen. Für eine zuverlässige Erfassung sind medienübergreifende Verfahren zu entwickeln, welche die drei analytischen Schritte, Probennahme, Probenaufbereitung und Detektion beinhalten. Die Verfahren adressieren unterschiedliche Zielgruppen, welche verschiedene analytische Informationen fordern. Für die akademische Bewertung werden Verfahren mit hohem analytischen Aufwand favorisiert, welche möglichst detaillierte Information über Partikelsorte, -größe, -zahl und -oberflächenbeschaffenheit geben. Im Gegensatz dazu, fordern Anwender aus der Praxis schnelle und einfache Monitoring Verfahren, welche die Bestimmung eines Massengehaltes, bzw. eines Grenzwertes zulassen. Allen ist gemeinsam, dass ein hoher interdisziplinärer Anspruch besteht, der sowohl technische Voraussetzungen zur repräsentativen Probennahme und die Limitationen von Detektionsverfahren berücksichtigt, als auch die Fachkompetenz von Biologen, Umweltwissenschaften, Analytiker und Polymerwissenschaftler einschließt. Verfahren zum Mikroplastiknachweis müssen auch verschieden Proben mit sehr unterschiedlichen Gehalten an natürlicher Matrix gerecht werden. So müssen allein für Wasser Verfahren entwickelt werden, die Mikroplastik verschiedener Form (sphärische Partikel, komplexe Bruchstücke, Fasern) aus Medien mit sehr variablen Partikelanteil (u.a. Trinkwasser, Oberflächenwasser, Abwasser) repräsentativ erfassen, sowie schnell und kostengünstig sind – einschließlich der notwendigen Probenaufbereitung. Die jeweiligen Detektionsverfahren müssen z.B. einzelne Partikel oder integrale Gehalte über drei Dekadenklassen für thermoplastische und insbesondere auch elastomere Partikelsorten erfassen können. T2 - GDCh Wissenschaftsforum CY - Aachen, Germany DA - 15.09.2019 KW - Mikroplastik KW - Analytik KW - TED-GC-MS PY - 2019 AN - OPUS4-49068 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaeger, Carsten T1 - Improving Small Molecule Annotation In Nontargeted Soft Ionization GC/LC High Resolution Mass Spectrometry N2 - High-resolution mass spectrometry, either combined with gas or liquid chromatography (GC/LC-HR-MS), is currently the most powerful analytical option for broad nontargeted small molecule analysis. To transform HR-MS raw data from metabolomics or environmental studies into chemically meaningful data, several computational steps are needed, including peak detection, deconvolution of these peaks into compounds and putative identification of compounds using databases. Each of these steps can cause problems and still requires methodological advancements. Computational compound annotation as one of the steps, however, has proven particularly challenging, mainly due to the chemical diversity of organic analytes. In addition, different annotation approaches are needed for the different platforms used in HR-MS screening. We recently introduced InterpretMSSpectrum as an annotation workflow for GC-HR-MS using atmospheric pressure chemical ionization (APCI). InterpretMSSpectrum locates molecular ion, fragment and adduct peaks, calculates their most likely sum formula combination and graphically summarizes results as an annotated mass spectrum. As a complementary approach for LC-HR-MS, we presented findMAIN, which scores MS1 spectra based on explained intensity, mass accuracy and isotope charge agreement of adducts and related electrospray ionization (ESI) products to determine the neutral mass of unknown compounds. Both approaches were validated against large spectral libraries containing more than 600 compounds, for which correct annotation was achieved in over 80% of the cases. Based on the experiences from this validation, we here compare soft-ionization GC/LC-HR-MS regarding “annotatability” of unknown compounds from a computational perspective. As a main advantage for GC-HR-MS, the relatively uniform ionization behavior of commonly used trimethylsilyl (TMS) derivatives observed under APCI allowed differentiation of molecular ion peaks from in-source fragments based on relatively compact set of rules. By contrast, neutral mass inference in ESI required a more complex evaluation scheme, due to the higher diversity of ionization products observable in ESI. We demonstrate such differences by practical examples of both software packages applied to metabolomics studies and discuss the challenges connected to transferring the approaches to environmental screening. T2 - ACS Fall Meeting 2019 CY - San Diego, CA, USA DA - 25.09.2019 KW - Compound annotation KW - Mass spectrometry KW - Electrospray ionization KW - Nontarget analysis KW - Accurate mass PY - 2019 AN - OPUS4-49200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian A1 - Koch, Matthias A1 - Kühn, S. A1 - Haase, H. T1 - Measuring the sum – A novel screening method for ergot alkaloids in food N2 - Ergot alkaloids play a significant role in human history for more than 1000 years and are part of the most common contaminants of food and feed worldwide. Their high toxicity against humans and livestock even at low concentrations causes a high demand for quick and reliable analytics even though no European limits for ergot alkaloids have been determined yet. Currently the most common methods for the quantitation of the six major ergot alkaloids and their corresponding stereoisomers are HPLC based, using either fluorescence or mass spectrometric detection. Whereas these conventional detection methods measure each compound individually, a novel approach is to transfer all ergot alkaloids to one basic structure, which could be measured as a sum parameter. Since all ergots contain a lysergic acid amide moiety and a differing peptide component, cleaving the molecule into a simple lysergic acid derivative, which could be quantified via either HPLC-FLD or MS/MS, is intended. To clean up the cleavage reaction mixture molecularly imprinted polymers (MIPs) are a simple and effective way to separate the desired structure. Due to the selectivity of MIPs, an improved matrix separation is expected, which results in fewer interferences in the FLD and the possibility to measure samples with more complex matrices. When fully developed, the novel method could overcome some major drawbacks of the conventional detection methods. Higher throughput and the need for less well-trained personnel are just two advantages, that should lead to a quick and cheap quantitation of ergot alkaloids. First results of this project will be presented, funded by the German ZIM program (Zentrales Innovationsprogramm Mittelstand) of the Federal Ministry for Economic Affairs and Energy. T2 - WMFmeetsIUPAC 2019 CY - Belfast, UK DA - 14.10.2019 KW - Ergot KW - Mycotoxins KW - Molecularly imprinted polymers PY - 2019 AN - OPUS4-49436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian A1 - Koch, Matthias A1 - Haase, H. A1 - Kühn, S. T1 - Measuring the sum – A novel screening method for ergot alkaloids in food N2 - Ergot alkaloids play a significant role in human history for more than 1000 years and are part of the most common contaminants of food and feed worldwide. Their high toxicity against humans and livestock even at low concentrations causes a high demand for quick and reliable analytics even though no European limits for ergot alkaloids have been determined yet. Currently the most common methods for the quantitation of the six major ergot alkaloids and their corresponding stereoisomers are HPLC based, using either fluorescence or mass spectrometric detection. Whereas these conventional detection methods measure each compound individually, a novel approach is to transfer all ergot alkaloids to one basic structure, which could be measured as a sum parameter. Since all ergots contain a lysergic acid amide moiety and a differing peptide component, cleaving the molecule into a simple lysergic acid derivative, which could be quantified via either HPLC-FLD or MS/MS, is intended. To clean up the cleavage reaction mixture molecularly imprinted polymers (MIPs) are a simple and effective way to separate the desired structure. Due to the selectivity of MIPs, an improved matrix separation is expected, which results in fewer interferences in the FLD and the possibility to measure samples with more complex matrices. When fully developed, the novel method could overcome some major drawbacks of the conventional detection methods. Higher throughput and the need for less well-trained personnel are just two advantages, that should lead to a quick and cheap quantitation of ergot alkaloids. First results of this project will be presented, funded by the German ZIM program (Zentrales Innovationsprogramm Mittelstand) of the Federal Ministry for Economic Affairs and Energy. T2 - WMFmeetsIUPAC 2019 CY - Belfast, UK DA - 14.10.2019 KW - Ergot KW - Mycotoxins KW - Molecularly imprinted polymers PY - 2019 AN - OPUS4-49437 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 - PharmaGlass Workshop CY - Sheffield, UK DA - 09.10.2019 KW - CRM KW - Hydrolytic resistance KW - Borosilicate glass PY - 2019 AN - OPUS4-49466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sebald, M.A. A1 - Gebauer, J. A1 - Sommerfeld, Thomas A1 - Koch, Matthias T1 - First Synthesis of (−)-Altenuene-D3 Suitable as Internal Standard for Isotope Dilution Mass Spectrometry N2 - Metabolites from Alternaria fungi exhibit a variety of biological properties such as phytotoxic, cytotoxic, or antimicrobial activity. Optimization of a literature procedure culminated in an efficient total synthesis of (−)-altenuene as well as a stable isotope-labeled derivative suitable for implementation in a LC-MS/MS method for mycotoxin analysis. KW - Altenuene KW - Alternaria mycotoxins KW - Food safety KW - Isotope-labeled KW - SIDA-LC-MS/MS KW - Suzuki coupling PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500696 DO - https://doi.org/10.3390/molecules24244563 SN - 1420-3049 VL - 24 SP - 4563 PB - MDPI CY - Basel AN - OPUS4-50069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Faßbender, Sebastian A1 - Rodiouchkina, K. A1 - Vanhaecke, F. A1 - Meermann, Björn T1 - On-line hyphenation of CE with multicollector-ICP-MS for species-specific isotopic analysis of sulfur 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 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 future field could be species-specific isotopic analysis of biomolecules, as sulfur is the only covalently bound constituent of proteins which can be analyzed by MC-ICP-MS. T2 - CE-Forum 2019 CY - Waldbronn, Germany DA - 11.12.2019 KW - Isotopic analysis KW - Multicollector-ICP-MS KW - Capillary electrophoresis KW - Hyphenated techniques KW - Speciation analysis PY - 2019 AN - OPUS4-50038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Vacuum hot extraction: Detection of volatiles N2 - Der Vortrag gibt einen Überblick über die Möglichkete und Grenzen der Methode der Vakuum-Heiß-Extraktion an der BAM T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - Berlin, Germany DA - 25.01.2019 KW - Heißgasextraktion KW - Glas PY - 2019 AN - OPUS4-50434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Bestimmung von Nichtmetallen in Carbiden N2 - Vortrag zur Bestimmung von Nichtmetallen in Carbiden halten. Hierbei geht es um die Bestimmung von C, O und N in Vanadiumcarbid, Wolframcarbid und Niobcarbidmaterialien, einen hierzu durchgeführten Ringversuch mit Beteiligung der Kollegen des AK Sonderwerkstoffe und den Vergleich von Verfahrenskenngrößen. T2 - Vollversammlung Chemikerausschuss der GDMB CY - Kassel, Germany DA - 05.11.2019 KW - Niobcarbid KW - Wolframcarbid KW - Vanadiumcarbid KW - Nichtmetalle PY - 2019 AN - OPUS4-50261 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kneipp, Janina A1 - Zancajo, Victor M.R. A1 - Diehn, S. A1 - Filiba, N. A1 - Elbaum, R. T1 - Spectroscopic Discrimination of Sorghum Silica Phytoliths N2 - Grasses accumulate silicon in the form of silicic acid, which is precipitated as amorphous silica in microscopic particles termed phytoliths. These particles comprise a variety of morphologies according to the cell type in which the silica was deposited. Despite the evident morphological differences, phytolith chemistry has mostly been analysed in bulk samples, neglecting differences between the varied types formed in the same species. In this work, we extracted leaf phytoliths from mature plants of Sorghum bicolor (L.) Moench. Using solid state NMR and thermogravimetric analysis, we show that the extraction methods alter greatly the silica molecular structure, its condensation degree and the trapped organic matter. Measurements of individual phytoliths by Raman and synchrotron FTIR microspectroscopies in combination with multivariate analysis separated bilobate silica cells from prickles and long cells, based on the silica molecular structures and the fraction and composition of occluded organic matter. The variations in structure and composition of sorghum phytoliths suggest that the biological pathways leading to silica deposition vary between these cell types. KW - Phytoliths KW - Biosilicification KW - Raman KW - Sorghum KW - Solid state NMR KW - Synchrotron FTIR PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502672 DO - https://doi.org/10.3389/fpls.2019.01571 VL - 10 SP - 1571 PB - Frontiers Media CY - Lausanne AN - OPUS4-50267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Koellensperger, G. A1 - Theiner, S. A1 - Schweikert, A. A1 - Flemig, Sabine A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - Quantitative Imaging of Silver Nanoparticles and Essential Elements in Thin Sections of Fibroblast Multicellular Spheroids by High Resolution Laser Ablation Inductively Coupled Plasma Time-of-Flight Mass Spectrometry N2 - We applied high resolution laser ablation inductively coupled plasma time-of-flight mass spectrometry (LA-ICP-TOF-MS) with cellular spatial resolution for bioimaging of nanoparticles uptaken by fibroblast multicellular spheroids (MCS). This was used to quantitatively investigate interactions of silver nanoparticles (Ag NPs) and the distributions of intrinsic minerals and biologically relevant elements within thin sections of a fibroblast MCS as a three-dimensional in vitro tissue model. We designed matrix-matched calibration standards for this purpose and printed them using a noncontact piezo-driven array spotter with a Ag NP suspension and multielement standards. The limits of detection for Ag, Mg, P, K, Mn, Fe, Co, Cu, and Zn were at the femtogram (fg) level, which is sufficient to investigate intrinsic minerals in thin MCS sections (20 μm thick). After incubation for 48 h, Ag NPs were enriched in the outer rim of the MCS but not detected in the core. The localization of Ag NPs was inhomogeneous in the outer rim, and they were colocalized with a single-cell-like structure visualized by Fe distribution (pixel size of elemental images: 5 × 0.5 μm). The quantitative value for the total mass of Ag NPs in a thin section by the present method agreed with that obtained by ICP-sector field (SF)-MS with a liquid mode after acid digestion. KW - Laser ablation KW - ICP-MS KW - Imaging KW - Nanoparticle KW - Cell KW - Spheroid PY - 2019 UR - https://pubs.acs.org/doi/10.1021/acs.analchem.9b02239 DO - https://doi.org/10.1021/acs.analchem.9b02239 SN - 0003-2700 VL - 91 IS - 15 SP - 10197 EP - 10203 PB - American Chemical Society, ACS Publications CY - Washington D.C. AN - OPUS4-48719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Paz, B. A1 - Völling, E. T1 - On the ore provenance of the Trojan silver artefacts N2 - Lead isotopes are a well-established tool to trace the geographic origin of samples and artefacts in archaeology and geochemistry. In archaeology, lead isotopes are often applied to gain information on the provenance of the used ores especially in lead and silver artefacts. The assignment of a specific and unambiguous provenance in most cases is not possible or at least hindered due to several limitations such as ore deposits overlapping in their lead isotopic composition, a large spread within one ore deposit or a missing overlap with known mining sites. Such difficult cases can only be solved by using information from sources being independent of the isotope data. This information can be of chemical nature such as concentrations of key elements or they can be of archaeological nature such as cultural or trade route information.Within this study, we combined lead isotope data of ores and artefacts with silver mass fractions in the ore deposits, Au/Ag-ratios in ores and artefacts and finally archaeological Information on the cultural context in the Mediterranean and Anatolian Region. This approach enabled us to significantly reduce the potential number of mining regions. Finally, the potential sources could be narrowed down to the three remaining locations the Central Taurus, Arap Dağ and the Eastern Troad. Beneath these three locations, the Central Taurus shows the highest probability for the geographic origin of the galena which has been used to create the Trojan silver artefacts. KW - Trojan silver artefacts KW - Priam's treasure KW - Lead isotope composition KW - Central Taurus KW - Ore provenance KW - Elemental composition PY - 2019 DO - https://doi.org/10.1007/s12520-018-0756-x SN - 1866-9557 SN - 1866-9565 VL - 11 IS - 7 SP - 3267 EP - 3277 PB - Springer Verlag AN - OPUS4-48272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska T1 - Materials research with synchrotron radiation N2 - Synchrotron radiation sources with their unique properties in terms of intensity, polarization and adjustability offer a wide range of possibilities in materials research. A basic introduction about the creation and special properties of synchrotron radiation will be given. Examples of current work at BAMline, the high-energy measuring facility of the Federal Institute for Materials Research and Testing at the synchrotron BESSY, are used to illustrate the possibilities and limitations of existing measuring methods. It will be shown how the formation of corrosion layers can be tracked, how the abrasion of implants leads to the introduction of heavy metals into the surrounding bone matrix and how the detection of smallest impurities in gold is possible by optimizing the measuring conditions. Finally, an outlook at the hardware and software developments to be expected in the coming years is given. T2 - INCT-FNA Symposium 2019 CY - Niteroi, Brazil DA - 27.05.2019 KW - Synchrotron KW - XRF KW - XANES KW - EXAFS KW - TXRF KW - Color X-ray Camera PY - 2019 AN - OPUS4-48897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faßbender, Sebastian A1 - Döring, A.-K. A1 - Meermann, Björn T1 - Development of complementary CE-MS methods for speciation analysis of pyrithione-based antifouling agents N2 - In the recent decade, metal pyrithione complexes have become important biocides for antifouling purposes in shipping. The analysis of metal pyrithione complexes and their degradation products/species in environmental samples is challenging because they exhibit fast UV degradation, transmetalation, and ligand substitution and are known to be prone to spontaneous species transformation within a chromatographic system. The environmental properties of the pyrithione species, e.g., toxicity to target and non-target organisms, are differing strongly, and it is therefore inevitable to identify as well as quantify all species separately. To cope with the separation of metal pyrithione species with minimum species transformation during analysis, a capillary electrophoresis (CE)–based method was developed. The hyphenation of CE with selective electrospray ionization- and inductively coupled plasma–mass spectrometry (ESI-, ICP-MS) provided complementary molecular and elemental information for the identification and quantification of pyrithione species. To study speciation of pyrithiones, a leaching experiment of several commercial antifouling paints containing zinc pyrithione in ultrapure and river water was conducted. Only the two species pyrithione (HPT) and dipyrithione ((PT)2) were found in the leaching media, in concentrations between 0.086 and 2.4 μM (HPT) and between 0.062 and 0.59 μM ((PT)2), depending on the paint and leaching medium. The limits of detection were 20 nM (HPT) and 10 nM ((PT)2). The results show that complementary CE-MS is a suitable tool for mechanistical studies concerning species transformation (e.g., degradation) and the identification of target species of metal pyrithione complexes in real surface water matrices, laying the ground for future environmental studies. KW - Complementary MS KW - Environmental speciation KW - Capillary electrophoresis-mass spectrometry KW - Antifouling biocides PY - 2019 DO - https://doi.org/10.1007/s00216-019-02094-5 SN - 1618-2642 VL - 411 IS - 27 SP - 7261 EP - 7272 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-48962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lopez-Serrano Oliver, Ana A1 - Haase, A. A1 - Peddinghaus, A. A1 - Wittke, D. A1 - Jakubowski, Norbert A1 - Luch, A. A1 - Grützkau, A. A1 - Baumgart, S. T1 - Mass cytometry enabling absolute and fast quantification of silver nanoparticle uptake at the single cell level N2 - In the last decades, significant efforts have been made to investigate possible cytotoxic effects of metallic nanoparticles (NPs). Methodologies enabling precise information regarding uptake and intracellular distribution of NPs at the single cell level remain to be established. Mass cytometry (MC) has been developed for high-dimensional single cell analyses and is a promising tool to quantify NP−cell interactions. Here, we aim to establish a new MC-based quantification procedure to receive absolute numbers of NPs per single cell by using a calibration that considers the specific transmission efficiency (TE) of suspended NPs. The current MC-quantification strategy accept TE values of complementary metal solutions. In this study, we demonstrate the different transmission behavior of 50 nm silver NPs (AgNP) and silver nitrate solution. We have used identical AgNPs for calibration as for in vitro-differentiated macrophages (THP-1 cell line) in a time- and dose-dependent manner. Our quantification relies on silver intensities measuring AgNPs in the same detection mode as the cells. Results were comparable with the TE quantification strategy using AgNPs but differed when using ionic silver. Furthermore, intact and digested cell aliquots were measured to investigate the impact of MC sample processing on the amount of AgNPs/cell. Taken together, we have provided a MC-specific calibration procedure to precisely calculate absolute numbers of NPs per single cell. Combined with its unique feature of multiplexing up to 50 parameters, MC provides much more information on the single cell level than single cell-inductively coupled plasma mass spectrometry (SC-ICP-MS) and, therefore, offers new opportunities in nanotoxicology. KW - ICP-MS KW - Nanoparticle KW - Cell KW - SC-ICP-MS KW - Mass cytometry PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b01870 SN - 0003-2700 SN - 1520-6882 VL - 91 IS - 18 SP - 11514 EP - 11519 PB - American Chemical Society (ACS Publications) CY - Washington AN - OPUS4-48986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Blind, K. T1 - Testbeds for standardization in the IIoT N2 - The poster presents our research findings on the role and impacts of testbeds in standardization for the industrial internet of things. Based on a multiple case study, four different approaches were identified followed in the testbeds with regard to their standardization activities. T2 - BRIDGIT2 conference at NSAI CY - Dublin, Irland DA - 11.09.2019 KW - IIoT KW - Normen KW - Industrie 4.0 KW - Standards KW - Normung KW - Standardization KW - Testbed PY - 2019 AN - OPUS4-48937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Koellensperger, G. A1 - Theiner, S. A1 - Schweikert, A. A1 - Flemig, Sabine A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - Imaging of Ag NP transport through collagen-rich microstructures in fibroblast multicellular spheroids by high-resolution laser ablation inductively coupled plasma time-of-flight mass spectrometry N2 - We investigated the penetration of silver nanoparticles (Ag NPs) into a three-dimensional in vitro tissue analog using NPs with various sizes and surface coatings, and with different incubation times. A high-Resolution laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) time-of-flight (TOF) instrument was applied for imaging the distributions of elements in thin sample sections (20 μm thick). A fibroblast multicellular spheroid (MCS) was selected as the model system and cultured for more than 8 days to produce a natural barrier formed by the extracellular matrix containing collagen. The MCS was then exposed for up to 48 h to one of four types of Ag NPs (∅ 5 nm citrate coated, ∅ 20 nm citrate coated, ∅ 20 nm polyvinylpyrrolidone coated, and ∅ 50 nm citrate coated). Imaging showed that the penetration pathway was strongly related to steric networks formed by collagen fibrils, and Ag NPs with a hydrodynamic diameter of more than 41 nm were completely trapped in an outer rim of the MCSs even after incubation for 48 h. In addition, we examined the impact of these NPs on essential elements (P, Fe, Cu, and Zn) in areas of Ag NP accumulation. We observed a linear increase at the sub-femtogram level in the total concentration of Cu (fg per pixel) in samples treated with small or large Ag NPs (∅ 5 nm or ∅ 50 nm) for 48 h. KW - Nanoparticle KW - Laser ablation KW - ICP-MS KW - Imaging KW - Cell PY - 2019 DO - https://doi.org/10.1039/c9an00856j SN - 0003-2654 VL - 144 IS - 16 SP - 4935 EP - 4942 PB - Royal Society of Chemistry RSC CY - Cambridge AN - OPUS4-48531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Schwinn, M. A1 - Kuhlmeier, K. A1 - Büchel, C. A1 - Meermann, Björn T1 - Development of an automated on-line purification HPLC single cell-ICP-MS approach for fast diatom analysis N2 - The most challenging part in performing a single cell ICP-MS (sc-ICP-MS) approach is the sample preparation, in particular the reduction of the ionic background. This step is, in many cases, time-consuming and required for each sample separately. Furthermore, sc-ICP-MS measurements are mostly carried out "manually", given the fact that present systems are not allowing for an automated change of samples. Thus, within this work, we developed an approach based on a HPLC system coupled on-line with sc-ICP-MS via a set of switching valves as well as an in-line filter for automated cell washing. This set-up enables the ionic background removal as well as analysis of single cells completely automated without any manual sample pretreatment. Our approach was applied for the analysis of the single celled diatom species Cyclotella meneghiniana, a marine diatom species, on the basis of Mg24 and facilitates testing in 11 min per sample, requiring only around 10,000 cells in a volume of 10 µL and approx. 10 mL of a 5% MeOH/95% deionized water (v/v) mixture. Even at extremely saline culturing media concentrations (up to 1000 mg L-1 magnesium) our on-line approach worked sufficiently allowing for distinction of ionic and particulate fractions. Furthermore, a set of diatom samples was analyzed completely automated without the need for changing samples manually. So, utilizing this approach enables analyzing a high quantity of samples in a short time and therefore in future the investigation of ecotoxicological effects is simplified for example in terms of metal accumulation by taking biovariability into account. KW - Single cell-ICP-MS KW - Diatoms KW - Ecotoxicology testing KW - Automated system PY - 2019 DO - https://doi.org/10.1016/j.aca.2019.05.045 SN - 1873-4324 VL - 1077 SP - 87 EP - 94 PB - Elsevier AN - OPUS4-48567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Lisec, Jan A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - Prediction of transformation products of monensin by electrochemistry compared to microsomal assay and hydrolysis N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for animal health, food, and environmental matters. The active agent Monensin (MON) belongs to the ionophore antibiotics and is widely used as a veterinary drug against coccidiosis in broiler farming. However, no electrochemically (EC) generated TPs of MON have been described so far. In this study, the online coupling of EC and mass spectrometry (MS) was used for the generation of oxidative TPs. EC-conditions were optimized with respect to working electrode material, solvent, modifier, and potential polarity. Subsequent LC/HRMS (liquid chromatography/high resolution mass spectrometry) and MS/MS experiments were performed to identify the structures of derived TPs by a suspected target analysis. The obtained EC-results were compared to TPs observed in metabolism tests with microsomes and hydrolysis experiments of MON. Five previously undescribed TPs of MON were identified in our EC/MS based study and one TP, which was already known from literature and found by a microsomal assay, could be confirmed. Two and three further TPs were found as products in microsomal tests and following hydrolysis, respectively. We found decarboxylation, O-demethylation and acid-catalyzed ring-opening reactions to be the major mechanisms of MON transformation. KW - Transformation products KW - Monensin KW - Veterinary drugs KW - Electrochemistry KW - Hydrolysis KW - LC/HRMS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485689 DO - https://doi.org/10.3390/molecules24152732 SN - 1420-3049 VL - 24 IS - 15 SP - 2732, 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-48568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - How to write your thesis N2 - Useful tips & tricks to overcome procrastination and get you PhD thesis written. T2 - 13. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 19.03.2019 KW - Outreach KW - Pomodore KW - Deep work PY - 2019 AN - OPUS4-48097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trimpin, S. A1 - Inutan, E. A1 - Karki, S. A1 - Elia, E. A1 - Zhang, W. A1 - Weidner, Steffen A1 - Marshall, D. A1 - Hoang, K. A1 - Lee, C. A1 - Davis, E. A1 - Smith, V. A1 - Meher, A. A1 - Cornejo, M. A1 - Auner, G. A1 - McEwen, C. T1 - Fundamental studies of new ionization technologies and insights from IMS-MS N2 - Exceptional ion mobility spectrometry mass spectrometry (IMS-MS) developments by von Helden, Jarrold, and Clemmer provided technology that gives a view of chemical/biological compositions previously not achievable. The ionization method of choice used with IMS-MS has been electrospray ionization (ESI). In this Special issue contribution, we focus on fundamentals of heretofore unprecedented means for transferring volatile and nonvolatile compounds into gas-phase ions singly and multiply charged. These newer ionization processes frequently lead to different selectivity relative to ESI and, together with IMS-MS, may provide a more comprehensive view of chemical compositions directly from their original Environment such as surfaces, e.g., tissue. Similarities of results using solvent- and matrix-assisted ionization are highlighted, as are differences between ESI and the inlet ionization methods, especially with mixtures such as bacterial extracts. Selectivity using different matrices is discussed, as are results which add to our fundamental knowledge of inlet ionization as well as pose additional avenues for inquiry. IMS-MS provides an opportunity for comparison studies relative to ESI and will prove valuable using the new ionization technologies for direct analyses. Our hypothesis is that some ESI-IMS-MS applications will be replaced by the new ionization processes and by understanding mechanistic aspects to aid enhanced source and method developments this will be hastened. KW - Inlet ionization KW - Vacuum ionization KW - Matrices KW - Fundamentals KW - Ion mobility PY - 2019 DO - https://doi.org/10.1007/s13361-019-02194-7 SN - 1044-0305 SN - 1879-1123 VL - 30 IS - 6 SP - 1133 EP - 1147 PB - Springer AN - OPUS4-48011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Prinz, Carsten A1 - Scholz, Gudrun A1 - Kemnitz, Erhard A1 - Emmerling, Franziska T1 - Ca-, Sr-, and Ba-Coordination polymers based on anthranilic acid via mechanochemistry N2 - Ca-, Sr-, and Ba-Based coordination polymers (CPs) were prepared mechanochemically by milling metal-hydroxide samples with anthranilic acid (oABAH). {[Ca(oABA)2(H2O)3]}n consists of one-dimensional polymeric chains that are further connected by a hydrogen-bonding network. {[Sr(oABA)2(H2O)2]·H2O}n is a one-dimensional CP in which water molecules bridge Sr2+ ions and increase the dimensionality by building an extended network. {[Ba(oABA)2(H2O)]}n crystallizes as a two-dimensional CP comprising one bridging water molecule. The cation radii influence the inorganic connectivity and dimensionality of the resulting crystal structures. The crystal structures were refined from powder X-ray diffraction data using the Rietveld method. The local coordination environments were studied via extended X-ray absorption fine structure (EXAFS) measurements. The compounds were further characterized using comprehensive analytical methods such as elemental analysis, thermal analysis, MAS NMR, imaging, and dynamic vapor sorption (DVS) measurements. Compounds 1, 2, and 3 exhibit small surface areas which decrease further after thermal annealing experiments. All compounds exhibit a phase transformation upon heating, which is only reversible in 3. KW - Mechanochemistry KW - XRD PY - 2019 DO - https://doi.org/10.1039/c9dt00991d SN - 1477-9226 SN - 1477-9234 VL - 48 IS - 19 SP - 6513 EP - 6521 PB - Royal Society of Chemistry AN - OPUS4-48014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred A1 - Seneschal-Merz, Karine A1 - Feldmann, Ines A1 - Bücker, Michael A1 - Oleszczuk, S. T1 - EDX-Analysis on medieval glasses and innovative protection of stained glass panels N2 - The church of Koszewko (Poland) is a brick building edified in the 15th century built on cobblestone foundations. There are five windows in the sanctuary. Three of them enclose heraldic panels from the Küssow’s family from the 15th century which are surrounded with Goethe glass from the 18th century to complete the windows. The colored heraldic panels are strongly damaged and corroded with massive paint layer losses, glass- and leadbreakages. Those medieval glass fragments have been shortly discovered and are of particular interest for Poland since only few medieval glazing have been conserved. The damages as well as the glass compositions have been investigated with ESEM/EDX. Two categories of medieval glass compositions have been identified. The blue glass is particularly sensible to corrosion because of his high content in K2O. The colorless and the red glass samples belong to a stable glass type. Due to the thickness of the gel layer, it is easy to see that the degradation is strongly proceeded. The protection of those medieval stained-glass panels is absolute necessary. The medieval panels have been restored and surrounded from a copper frame. Then they have been fixed on the wood frame in the church. The exterior glazing has been closed with a panel of Goethe glass. The gap between the Goethe- and the medieval glass is about 3 cm. The Goethe glass panel has been stabilized with a film based on polyester to protect the medieval glasses against any damages. In this way, a low cost protective glazing has been installed for a long-term conservation of each medieval stained-glass panels. The climate measurements over the period of one year on the restored windows are in process. The temperature and the relative humidity are recorded in the church interior, in the gap between the original and the Goethe glass and outdoors. T2 - 93rd Annual Meeting of DGG and Annual Meeting of USTV CY - Nuremberg, Germany DA - 13.05.2019 KW - Medieval glasses KW - Stained glasses KW - EDX Analysis KW - Corrosion PY - 2019 AN - OPUS4-48025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lörchner, Dominique A1 - Dittmann, Daniel A1 - Braun, Ulrike A1 - Kroh, L. W. A1 - Köppen, Robert T1 - Investigation of two triazine-based heterocyclic brominated flame retardants by coupled thermogravimetry-Fourier transform infrared spectroscopy N2 - In this study, the thermal decomposition of 1,3,5-tris-(2,3-dibromopropyl)-1,3,5-triazine-2,4,6-trione (TDBPTAZTO) and 2,4,6-tris-(2,4,6-tribromo-phenoxy)-1,3,5-triazine (TTBP-TAZ) were investigated for the first time by thermogravimetric analysis. Both compounds were thermal degraded between 225 and 350 °C (TDBP-TAZTO) as well as 300 and 400 °C (TTBP-TAZ). As a result, mass loss (%) of 98.5% for TTBP-TAZ and 95.4% for TDBP-TAZTO at 600 °C under N2 were observed. The major pyrolytic degradation products of TTBP-TAZ were formed in a single step and identified by FTIR analysis as 2,4,6-tribromophenol and further bromine-substituted aromatic compounds. In comparison, TDBP-TAZTO was pyrolytic degraded in two steps, whereby on the first step the release of hydrogen Bromide and 1,3,5-triallyl-1,3,5-triazine-2,4,6-trione could be detected. In the second minor step, isocyanic acid could be additionally identified. Subsequently, the obtained products of the TGA-FTIR measurements were used for a targeted search for mass fragments in mass spectrometry measurements. For TTBP-TAZ, only the degradation product 1,3,5-tribromobenzene could be detected by MS/MS analyzes. No comparable thermal degradation products, except hydrogen bromide, were observed in the MS/MS spectra of TDBP-TAZTO. Therefore, the search of further mass fragments was not possible compared to the findings of the TGA-FTIR measurements. KW - Pyrolysis KW - Thermal decomposition KW - TGA-FTIR KW - Mass spectrometry PY - 2019 DO - https://doi.org/10.1016/j.jaap.2019.104635 VL - 141 SP - 104635-1 EP - 104635-5 PB - Elsevier B.V. AN - OPUS4-48506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Flemig, Sabine A1 - Koellensperger, G. A1 - Theiner, S. A1 - Schweikert, A. A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - Localization of cells and exposed nanoparticles in three-dimensional in vitro tissue analog measured by means of an elemental microscopy based on LA-ICP-TOF-MS N2 - Metallic nanoparticles (NPs) are currently applied in a variety of consumer products and are also attractive for medical applications. With their widespread use, the potential for human exposure to NPs — either intended or unintended — is increasing. Therefore, many studies have evaluated the toxicity and transport mechanism of NPs. In comparison with two-dimensional cultured cells, multicellular spheroids (MCS) look promising to be used as a three-dimensional cellular model, having unique advantages in nanoparticle studies due to the fact that interactions with excreted extracellular matrix can be investigated. Fibroblast cells are one of the most important cell systems to express a microenvironment by excreting an abundant extracellular matrix. For bioimaging laser ablation inductively coupled-plasma mass spectrometry (LA-ICP-MS) is used in this investigation to study the interaction of metallic NPs with MCS for multi-element detection offering a wide dynamic range. As a mass spectrometer we have applied a time-of-flight (TOF) instrument for (quasi-) simultaneous detection of all isotopes of elements of interest. The aim of this study is to investigate the localization of silver (Ag) NPs exposed to fibroblast MCSs by means of LA-ICP-TOF-MS. In addition, for demonstrating elemental microscopy we chose phosphorous (31P) and iron (56Fe) to visualize regions of enriched extracellular matrix and single cells, respectively. In this presentation, we show that exposed Ag NPs are highly accumulated at the same position of single cells in an outer rim of fibroblast MCSs. T2 - 7th International Symposium on Metallomics CY - Warsaw, Poland DA - 30.06.2019 KW - Nanoparticle KW - Laser ablation KW - ICP-MS KW - Multicellular spheroid PY - 2019 AN - OPUS4-48425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaeger, Carsten A1 - Lisec, Jan T1 - Rapid characterization of ionization products for chemistry-aware compound annotation in nontargeted small molecule mass spectrometry N2 - Nontargeted high-resolution mass spectrometry (HRMS) is widely used for small molecule screening in biotic or abiotic samples. However, HRMS approaches like metabolomics or environmental nontarget screening currently still lack confidence in chemical annotation, i.e. computational structure assignment to all measured mass signals. As a crucial step within the annotation pipeline, molecular weight inference (MWI) deduces a compound’s intact mass from diagnostic mass differences between MS1 peaks, allowing precise database queries in subsequent steps. As the common practice of considering all possible ionization products such as adducts, multimers, multiple charges etc. in MWI suffers from high false positive rates, we aimed at selecting candidate ionization products in a chemically sensitive way. Generally, electrospray ionization produces different types of adducts depending on chromatographic system and sample matrix, necessitating application-specific optimization for optimum MWI performance. To avoid, however, the tedious and potentially biased manual data curation connected to optimization, we established an R-based workflow for automating this task. The workflow consists of two parts. Part 1 creates an MS1 spectral library by performing peak detection, spectral deconvolution and target peak assignment based on density estimation. Part 2 analyzes ion relationships within the library and returns a list of detected ionization products ranked by their frequency. We applied the workflow to a commercial 634-compound library that was acquired for two chromatographic methods (reverse phase, RP; hydrophilic liquid interaction chromatographic, HILIC) and the two ESI modes (positive, negative). As expected, different frequency distributions of ionization products were found for the two chromatographies. Interestingly, however, some of the differences were expected in terms of solvent chemistries (e.g. [M+NH4]+ in ammonium formate-buffered HILIC) while others indicated more complex ion competition (e.g. abundant [M+K]+, [M+2K-H]+ in HILIC). This demonstrated the relevance of this empirical approach. We further show that MWI accuracy clearly benefitted from derived optimized adduct lists – by adding filters or weighting terms – and present FDR calculations supporting this observation. We conclude that chemistry-aware compound annotation based on the combination of high-throughput library acquisition and statistical analysis holds significant potential for further improvements in nontargeted small molecule HRMS. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Compound annotation KW - Mass spectrometry KW - Electrospray ionization KW - Nontarget analysis KW - Accurate mass PY - 2019 AN - OPUS4-48332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaeger, Carsten T1 - Comparing Nontargeted LC-MS Methods by Co-visualizing Linear Dynamic Range and Chemical Coverage N2 - INTRODUCTION Biological and environmental samples contain thousands of small molecule species that all vary in chemical properties and concentration range. Identifying and quantifying all these chemical entities remains a long-term goal in metabolomics and related systems approaches. Due to its broad selectivity, nontargeted LC-MS is usually the method of choice for broad chemical screening. Optimizing nontargeted LC-MS methods, however, is less straightforward than for targeted methods where sensitivity, specificity, linearity etc. serve as well-established performance criteria. We therefore investigated linear dynamic range (LDR) and chemical classification as alternative performance criteria to guide nontargeted method development. EXPERIMENTAL METHODS LDR was defined as the linear portion of a feature’s response curve over multiple concentration levels. Comparing the LDR of features across methods can be expected to be significantly more robust than comparing signal intensities for a single concentration. To determine LDR for all features, a computational workflow was implemented in the R programming language. For estimating the linear portion of a curve, several mathematical approaches including linear, non-linear and piecewise linear regression were evaluated. Chemical classification was based on ClassyFire, which computes chemical classes for a given structure. To avoid false classifications for incorrectly annotated compounds, we took the following statistical approach. For each compound, multiple likely annotation hypotheses were derived using a recently described workflow[2]. All annotation hypotheses were submitted to ClassyFire and obtained classifications were ranked by frequency. The most frequently suggested class was kept for further analysis. Finally, LDR and chemical classes were visualized together on a molecular network, which was constructed using the well-established MS/MS similarity approach. RESULTS AND DISCUSSION For technical validation of the workflow, several hundred curve fits obtained from the different regression models were reviewed visually. Piecewise linear regression performed the most reliably with respect to the heterogeneous curve shapes of ‘real-life’ features. Validation of chemical classification was performed against a compound library, which showed that 90% of ~450 library compounds were correctly classified using the described approach. Two liquid chromatography methods (HILIC, RPC) as well as two electrospray ionization variants (low/high-temperature ESI) applied to urinary metabolomics were exemplarily studied to test the workflow. Molecular network visualization indicated that of all analytical setups, HILIC/high temperature ESI performed best in terms of high LDR achieved over a wide range of compound classes. Despite one order of magnitude lower sensitivity, HILIC/low temperature ESI showed similar chemical coverage, except for organic nitrogen compounds that were underrepresented compared to high-temperature ESI. Both RPC setups were inferior to the HILIC setups in terms of high-LDR features, supporting previous findings for the given matrix. The higher relative representation of benzenoids and lipids in RPC demonstrated that the workflow successfully captured expected selectivity differences between chromatographies. CONCLUSION When comparing nontargeted LC-MS methods for optimization purposes, ideally all available quantitative and qualitative information should be integrated. The present workflow follows this idea. Visualizing LDR and chemical classes of all features on a molecular network quickly indicated differences in method selectivity that were otherwise difficult to spot. As an automated approach, it is easily applied to repeated optimization steps, enabling effective optimization strategies. T2 - EURACHEM Workshop CY - Tartu, Estonia DA - 20.05.2019 KW - Linear dynamic range KW - Liquid chromatography-mass spectrometry KW - Nontargeted approach KW - Method development KW - Chemical coverage PY - 2019 AN - OPUS4-48333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pisonero, J. A1 - Fandino, J. A1 - Nordlien, J. H A1 - Richter, Silke A1 - Pfeifer, Jens A1 - Quarles, C. D. A1 - Gonzalez, J. A1 - Jakubowski, Norbert A1 - Bordel, N. T1 - Improving the analytical performance of pulsed-GD-SFMS for multi-elemental depth profile analysis of heat-treated Zn coatings on extruded aluminium N2 - The formation of diffusion layers on Zn layers deposited on Al substrates is mainly used to prevent corrosion effects. Evaluation of the influence exerted by different coating methodologies and heat treatments on the formation of these diffusion layers is of great interest for the aluminium industry. Particularly, multi-elemental in-depth distributions of major, minor and trace elements in Zn-coatings is highly demanded before and after heat treatments. A fast characterization of these materials require a direct solid analytical technique able to provide high sensitivity and high depth resolution. For this purpose, an improved analytical method based on the use of pulsed glow discharge sector field mass spectrometry (pulsed-GD-SFMS) is investigated. Glow discharge operating parameters (e.g. pulse duration, pulse frequency), glow discharge source design (e.g. flow tube lengths), and SFMS mass spectra acquisition conditions (e.g. integration time) are evaluated to achieve low sputtering rates, high mass spectra acquisition rates and improved depth resolution. At the optimize conditions Zn coatings deposited by arc-spray and electrodeposition are analysed before and after heat treatments to evaluate the diffusion of different key elements. Moreover, results are validated using femtosecond laser ablation (fs-LA)-ICP-MS, which provides additional information about the heterogeneous distribution of some elements in the Zn coatings. KW - GDMS KW - Pulsed-GD-SFMS KW - Depht profiling KW - Zn KW - Aluminium PY - 2019 DO - https://doi.org/10.1039/c9ja00189a VL - 34 IS - 11 SP - 2252 EP - 2260 PB - Royal Society of Chemistry CY - London AN - OPUS4-49451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Reference materials for non-metal analysis N2 - The procedure for certification of reference materials in BAM in accordance with the rules of ISO Guide 35 is described using examples. In addition, a comprehensive overview of reference materials for the analysis of non-metals oxygen, hydrogen, nitrogen, coal and sulfur is given. T2 - LECO Workshop: CHNOS determination in inorganic (high tec) materials CY - Berlin, Germany DA - 22.10.2019 KW - CRM KW - Non-metal analysis KW - ISO-Guide 35 KW - Reference materials PY - 2019 AN - OPUS4-49458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tillo, Adam A1 - Bartelmeß, Jürgen A1 - Chauhan, Vraj P. A1 - Bell, Jérémy A1 - Rurack, Knut T1 - Microfluidic Device for the Determination of Water Chlorination Levels Combining a Fluorescent meso-Enamine Boron Dipyrromethene Probe and a Microhydrocyclone for Gas Bubble Separation N2 - Chlorination procedures are commonly applied in swimming pool water and wastewater treatment, yet also in food, pharmaceutical, and paper production. The amount of chlorine in water needs to be strictly controlled to ensure efficient killing of pathogens but avoid the induction of negative health effects. Miniaturized microfluidic fluorescence sensors are an appealing approach here when aiming at online or at-site measurements. Two meso-enamine-substituted boron dipyrromethene (BODIPY) dyes were found to exhibit favorable indication properties, their reaction with hypochlorite leading to strong fluorescence enhancement. Real-time assays became possible after integration of these fluorescent probes with designed two-dimensional (2D) and three-dimensional (3D) microfluidic chips, incorporating a passive sinusoidal mixer and a microhydrocyclone, respectively. A comparison of the two microfluidic systems, including their abilities to prevent accumulation or circulation of microbubbles produced by the chemical indication reaction, showed excellent fluidic behavior for the microhydrocyclone-based device. After coupling to a miniaturized optical reader for fluorescence detection, the 2D microfluidic system showed a promising detection range of 0.04−0.5 mg L−1 while still being prone to bubble-induced fluctuations and suffering from considerably low signal gain. The microhydrocyclone-based system was distinctly more robust against gas bubbles, showed a higher signal gain, and allowed us to halve the limit of detection to 0.02 mg L−1. The use of the 3D system to quantify the chlorine content of swimming pool water samples for sensitive and quantitative chlorine monitoring was demonstrated. KW - Chlorine KW - BODIPY KW - Fluorescence KW - Micro-Hydrocyclone KW - Microfluidic Chip PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b03039 SN - 0003-2700 VL - 91 IS - 20 SP - 12980 EP - 12987 PB - American Chemical Society CY - Washington, DC AN - OPUS4-49393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate A1 - Hahn, Oliver A1 - Overgaauw, E. A1 - Danielewski, A. A1 - Giel, R. T1 - Analyse von Humboldt Codices aus Mizquiahuala im Vergleich zu Fragmenten in Mexiko und Paris N2 - Unter den von Humboldt in Amerika erworbenen Schriftstücken der Kolonialzeit findet sich eine Tributliste aus dem Jahr 1569, die der Otomí Bevölkerung aus dem Ort Mizquahuala im Staat Hidalgo/ Mexiko zugeordnet wird. Sie ist in Form eines Kalenders ausgeführt, Wochentage und verschiedene Produkte lassen sich unterscheiden. Eduard Seler beschreibt dieses Manuskript zusammen mit einer weiteren Tributliste, die in Inhalt und Zeichnung anders gestaltet ist, jedoch ebenfalls aus dieser Region stammt. Mit den für die Analyse von Manuskripten bewährten Untersuchungsmethoden werden Papier und Farbmittel identifiziert. Hierzu zählen Raman-, FTIR-, Röntgenfluoreszenz- und VIS- Spektroskopie. Charakteristisch für die Herstellung von schriftlichen Dokumenten in der Kolonialzeit von Amerika ist die Verwendung von indigenem Material wie Papier aus Baumrinde und Pflanzenfarben zusammen mit den aus Europa bekannten Materialien. Geklärt wird, welche Auswahl von Farbstoffen zur Herstellung der Dokumente genutzt wurde, die diese als Gruppe klassifizieren könnte. Die den beiden Fragmenten zugeordneten Farbmaterialien sowie formale und inhaltliche Aspekte lassen vermuten, dass zwei weitere Schriftstücke der Berliner Sammlung `Manuscripta Americana´, deren Herkunft nicht bekannt ist, mit ihnen in Beziehung gebracht werden können. Stilistisch gleiche Fragmente befinden sich zudem in Mexiko, Paris und den USA. Im Vergleich dieser Fragmente untereinander wird diskutiert, inwieweit die über die Materialanalyse identifizierten spezifischen Farbstoffe einen Hinweis auf eine gemeinsame lokale Herkunft zulassen. T2 - Jahrestagung Archäometrie und Denkmalpflege CY - Wien, Austria DA - 11.09.2019 KW - VIS- Spektroskopie KW - Humboldt Codices KW - RFA PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499192 SN - 0947-6229 VL - Sonderheft 9 SP - 186 EP - 189 CY - Bochum AN - OPUS4-49919 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Hein, Sebastian A1 - von Törne, Jannik Wipert A1 - Kaminski, Katja A1 - Klyk-Seitz, Urszula-Anna T1 - NSO-Heterozyklen – Zwischen Rattengift und Normung N2 - Warfarin als ein Vertreter der NSO-Hetereozyklen, ist seit den 1950er Jahren einer der bekanntesten Gerinnungshemmer. Beim Menschen wird es bis heute zur Vorbeugung von Thrombose und der Behandlung von Vorhofflimmern und Arrhythmie eingesetzt. Doch schon einige Jahre vor der FDA Zulassung als Medikament wurde es zur Bekämpfung von Nagetieren eingesetzt. Bis heute wurde es nur teilweise durch weitaus wirksamere antikoagulante Rodentizide (ARs) der zweiten Generation, sogenannte Superwarfarine, ersetzt. In der Fachliteratur finden sich zahlreiche Beispiele für sekundäre und tertiäre Vergiftung mit ARs bei Wildtieren und anderen Nichtzieltieren. Bisher ist relativ wenig über die Bioakkumulation, Persistenz und Toxizität von ARs und deren Transformationsprodukten (TPs) in der terrestrischen und aquatischen Umwelt, sowie der Nahrungskette bekannt. Um Einblicke in mögliche Transformations- und Abbauprozesse von Warfarin zu erhalten und um Umwelteinflüsse zu simulieren, wurde es in einer elektrochemischen Reaktorzelle oxidativ umgesetzt und mittels Massenspektrometrie analysiert. Hinsichtlich der Wasseraufbereitung in Kläranlagen wurden technisch relevante Simulationsverfahren wie Chlorung, UV-Bestrahlung und Ozonung angewendet um potentielle Eliminierungswege aufzuklären. Gebildete Transformationsprodukte wurden daher mittels unterschiedlicher chromatografischer Verfahren getrennt, massenspektrometrisch analysiert und verglichen. T2 - MS-Tage CY - Düsseldorf, Germany DA - 03.12.2019 KW - GC-MS KW - Warfarin KW - NSO-Heterozyklen PY - 2019 AN - OPUS4-49974 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Rosner, M. A1 - Henehan, M. J. A1 - Tütken, T. T1 - Triple Isotope Fractionation Exponents of Elements Measured by MC-ICP-MS - An Example of Mg N2 - In most chemical reactions, stable isotopes are fractionated in a mass-dependent manner, yielding correlated isotope ratios in elements with three or more stable isotopes. The proportionality between isotope ratios is set by the triple isotope fractionation exponent θ that can be determined precisely for, e.g., sulfur and oxygen by IRMS, but not for metal(loid) elements due to the lower precision of MC-ICP-MS analysis and smaller isotopic variations. Here, using Mg as a test case, we compute a complete metrologically robust uncertainty budget for apparent θ values and, with reference to this, present a new measurement Approach that reduces uncertainty on θ values by 30%. This approach, namely, direct educt-product bracketing (sample−sample bracketing), allows apparent θ values of metal(loid) isotopes to be determined precisely enough to distinguish slopes in three-isotope space. For the example of Mg, we assess appropriate quality Control standards for interference-to-signal ratios and Report apparent θ values of carbonate−seawater pairs. We determined apparent θ values for marine biogenic carbonates, where the foraminifera Globorotalia menardii yields 0.514 ± 0.005 (2 SD), the coral Porites, 0.515 ± 0.006 (2 SD), and two specimens of the giant clam Tridacna gigas, 0.508 ± 0.007 (2 SD) and 0.509 ± 0.006 (2 SD), documenting differences in the uptake pathway of Mg among marine calcifiers. The capability to measure apparent θ values more precisely adds a new dimension to metal(loid) δ values, with the potential to allow us to resolve different modes of fractionation in industrial and natural processes. KW - Isotope fractionation KW - Delta value KW - Biogenic carbonates KW - Calcification KW - Magnesium isotope ratios KW - Measurement uncertainty KW - Sample-sample bracketing PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b02699 VL - 91 IS - 22 SP - 14314 EP - 14322 PB - ACS Publications AN - OPUS4-49818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, H. A1 - Song, W. A1 - Gröninger, Delia A1 - Zhang, L. A1 - Lu, Y. A1 - Chan, K. S. A1 - Zhou, Z. A1 - Rurack, Knut A1 - Shen, Z. T1 - Real-time monitoring of newly acidified organelles during autophagy enabled by reaction-based BODIPY dyes N2 - Real-time monitoring of newly acidified organelles during autophagy in living cells is highly desirable for a better understanding of intracellular degradative processes. Herein, we describe a reaction-based boron dipyrromethene (BODIPY) dye containing strongly electron-withdrawing diethyl 2-cyanoacrylate groups at the α-positions. The probe exhibits intense red fluorescence in acidic organelles or the acidified cytosol while negligible fluorescence in other regions of the cell. The underlying mechanism is a nucleophilic reaction at the central meso-carbon of the indacene core, resulting in the loss of π-conjugation entailed by dramatic spectroscopic changes of more than 200 nm between its colorless, non-fluorescent leuco-BODIPY form and its red and brightly emitting form. The reversible transformation between red fluorescent BODIPY and leuco-BODIPY along with negligible cytotoxicity qualifies such dyes for rapid and direct intracellular lysosome imaging and cytosolic acidosis detection simultaneously without any washing step, enabling the real-time monitoring of newly acidified organelles during autophagy. KW - Autophagy KW - BODIPY KW - Fluorescence KW - Lysosome KW - Real-time imaging PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498358 UR - https://www.nature.com/articles/s42003-019-0682-1 DO - https://doi.org/10.1038/s42003-019-0682-1 SN - 23993642 VL - 2 SP - 442 PB - Nature Research CY - London AN - OPUS4-49835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica A1 - Traub, Heike A1 - Anderhalten, L. C. A1 - Infante-Duarte, C. T1 - Imaging mass cytometry for visualisation of neuroinflammation induced changes N2 - Multiple sclerosis (MS) is the most common acquired neurological disease affecting Young adults. It leads to myelin destruction and formation of lesions in the brain and permeabilization of the blood-brain barrier (BBB). Gadolinium based contrast agents (GBCA), used for diagnosis and monitoring by MRI, might accumulate in tissue, including brain. Using an animal model, application of linear and macrocyclic GBCA was investigated. Analysis was performed by laser ablation inductively coupled plasma (LA-ICP) MS. This method works as a bioimaging tool for sample thin sections and allows to identify regions of accumulated Gd in the samples. In healthy and diseased mice, inflammationmediated changes in the brain were investigated by application of GBCA. The mean objective is to understand the changes in inflamed tissue and correlate alterations of the BBB by LA-ICP-MS (Imaging Mass Cytometry). T2 - Colloquium Analytische Atomspektroskopie 2019 CY - Freiberg, Germany DA - 23.09.2019 KW - Bioimaging KW - LA-ICP-MS KW - Imaging Mass Cytometry KW - Gadolinium PY - 2019 AN - OPUS4-49853 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - von Törne, Jannik Wipert T1 - Identification of Transformation Products of Warfarin N2 - Warfarin, also known as Coumadin is one of the most popular anticoagulant drugs used as a therapeutic in humans to prevent thrombosis, atrial fibrosis, and fibrillation since the 1950s. Because of its ability to hinder blood from clotting by blocking vitamin K-depending carboxylation of blood clotting precursors, it is also used as a rodenticide worldwide. Until today it has been partially substituted by far more potent anticoagulant rodenticides (ARs), so-called superwarfarins. There are numerous references confirming secondary and tertiary poisoning in non-target-animals and wildlife like mammals, birds, and fish associated with ARs. Up to now relatively little is known about persistence and toxicity of transformation products of those AR in the environment and food chain. Herein, warfarin was chosen as a model compound to determine andelucidate TPs which are generated technically and under environment-like conditions. Such as the simulation of the oxidative phase I metabolism by implementing electrochemical flow cells coupled to mass spectrometry (MS). Obtained results are being compared to TPs generated by UVB-irradiation and ozonation. Analysis and separation of degradation products and TPs were achieved by a variety of gas- and liquid chromatographic techniques coupled to (high resolution) MS. T2 - Goldschmidt 2019 CY - Barcelona, Spain DA - 18.08.2019 KW - GC-MS KW - Warfarin KW - Transformations products PY - 2019 AN - OPUS4-49795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke A1 - Roethke, A. A1 - Rienitz, O. A1 - Matschat, Ralf A1 - Schiel, D. A1 - Jaehrling, R. A1 - Goerlitz, V. A1 - Kipphardt, Heinrich T1 - SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods N2 - Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM – 25 years ago – up to latest achievements in the field of inorganic analysis. KW - Metrology KW - SI Traceability KW - CCQM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496080 DO - https://doi.org/10.1088/1681-7575/ab5636 SN - 0026-1394 SN - 1681-7575 SP - 1 EP - 23 PB - IOP CY - Bristol AN - OPUS4-49608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke A1 - Pfeifer, Jens A1 - Dommaschk, M. A1 - Abad Andrade, Carlos Enrique A1 - Recknagel, Sebastian T1 - Bestimmung von halogen in Metallen mittels spektrometrischer Verfahren N2 - Die metallischen Verunreinigungen in Metallen lassen sich mittels hochauflösender Massenspektrometer relativ einfach ermitteln. Die Glimmentladungs-Massenspektrometrie (GD-MS) stellt hierfür eine schnelle Multielementmethode dar. Aufgrund ihrer höheren Anregungs- und Ionisationsenergien ist die Bestimmung von Nichtmetallen eine weit größere Herausforderung. Außerdem fehlt es an für die direkte Feststofftechnik notwendigen Kalibrierstandards z.B. in Form zertifizierter Referenzmaterialien. Für die quantitative Bestimmung von Verunreinigungen wurden mit Standards dotierte Pulverpresslinge und dotierte, gesinterte Materialien auf ihre Eignung als Kalibrierstandards für die GD-MS untersucht. Dabei kamen unterschiedliche Plasmabedingungen (gepulster/ kontinuierlicher Betrieb; verschiedene Plasmagase) zum Einsatz. Ein Überblick über analytische Kenngrößen und Grenzen der verwendeten Kalibrierstrategien wird gegeben. Zur Validierung des Verfahrens wurde die hochauflösende Continuum Source Absorptionsspektrometrie (HR-CS-MAAS) verwendet. Die analytische Nutzung der Molekül-absorptionsspektrometrie zur Bestimmung von Halogenen basiert auf der Bildung insitu-generierter zweiatomiger Moleküle (AlCl, GaF). Die entstehenden Molekülspektren werden im Echelle-Spektrometer aufgespalten und mittels CCD-Array detektiert, was eine sehr empfindliche Messung und präzise Quantifizierung ermöglicht. T2 - CANAS 2019 CY - Freiberg, Germany DA - 23.09.2019 KW - Halogene PY - 2019 AN - OPUS4-49610 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike A1 - Drescher, D. A1 - Büchner, T. A1 - Müller, L. A1 - Wanka, Antje A1 - Hösl, S. A1 - Ascher, Lena A1 - Cruz-Alonso, M. A1 - Pisonero, J. A1 - Kneipp, J. A1 - Jakubowski, Norbert T1 - Imaging of biological samples by LA-ICP-MS N2 - In recent years, elemental imaging of biological samples like tissue thin sections using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining more and more importance. Improvements concerning spatial resolution as well as signal-to-background ratio due to low-dispersion sample chambers make LA-ICP-MS also interesting for single cell analysis. To evaluate the interaction of nanoparticles (NPs) with cells LA-ICP-MS was applied for the imaging of individual cells. Our findings show, that NP aggregates can be localized within cellular compartments. The uptake efficiency depends strongly on the physico-chemical properties of the nanostructures (size, chemical composition, surface modification), as well as on the incubation conditions (concentration, time). Moreover, LA-ICP-MS is increasingly becoming an important complementary technique in bioanalysis by using element-tagging strategies to determine biomolecules indirectly. Based on the specific binding between antibodies and their corresponding antigens, proteins and peptides can be detected in tissue or cells using tagged antibodies. As artificial tags metal chelates loaded with lanthanides, polymer-based elemental tags or metal-containing nanoparticles can be used. Thereby LA-ICP-MS is a sensitive detection tool for multiplexed immuno-histochemistry of tissue and cell samples. Our results demonstrate the potential of LA-ICP-MS to investigate the distribution of naturally occurring elements, administered agents as well as biomolecules by using metal-tagged antibodies. T2 - Workshop on tandem LIBS/LA-ICP-MS 2019 CY - Berlin, Germany DA - 18.11.2019 KW - Laser ablation KW - ICP-MS KW - Nanoparticles KW - Imaging PY - 2019 AN - OPUS4-49704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Wichmann, K. A1 - Lauer, F. A1 - Tremel, W. A1 - Vanhaecke, F. A1 - von der Au, M. A1 - Schwinn, M. A1 - Borovinskaya, O. A1 - Büchel, C. A1 - Kuhlmeier, K. T1 - Neue ICP-MS basierte Methoden zur Analyse von Nano- und Mikropartikeln in der Umwelt N2 - In den vergangen Jahren hat das Umweltbewusstsein in der Bevölkerung stark zugenommen und somit auch das Interesse an der Vermeidung von anthropogenen (Schad-)Stoffen in der Umwelt. Eine (neue) Substanzklasse, deren Umweltauswirkungen noch nicht vollständig untersucht sind und die in den vergangenen Jahren immer mehr an Bedeutung gewonnen hat, sind (metallbasierte) Nanomaterialien. Im Gegensatz zu bspw. Elementspezies weisen Nanomaterialien eine Vielzahl von Eigenschaften auf und lassen sich nicht über nur ein Merkmal beschreiben - dies stellt eine große analytische Herausforderung dar. Hier haben sich vor allem die Feld-Fluss-Fraktionierung (AF4) und die single-particle-ICP-MS als leistungsstarke analytische Methoden herausgestellt. In (aquatischen) Umweltmatrizes (z.B. Oberflächengewässern) liegen neben artifiziellen auch natürliche Partikel vor, was eine weitere große Herausforderung für den Nachweis von Nanomaterialien darstellt. Neben dem Nachweis von anthropogenen Stoffen in der Umwelt ist zudem deren ökotoxikologische Bewertung wichtig. In der aquatischen Ökotoxikologie werden hierzu Testorganismen mit den jeweiligen Substanzen über die Wasserphase exponiert. Effektkonzentrationen (EC50) werden dabei auf Basis der Konzentrationen in der Wasserphase abgeleitet - tatsächlich bioakkumulierte Mengen werden hierbei jedoch meist nicht ermittelt; eine weitere große Herausforderung besteht zudem in der Bewertung von Mischungstoxizitäten. Gängige Testorganismen sind u.a. Kieselalgen (Diatomeen). Diatomeen stehen am Anfang der Nahrungskette - toxikologisch relevante Metalle/Nanomaterialien können sich hierüber im Nahrungsnetz der Oberflächengewässer anreichern und ggf. nachhaltig auswirken. Im ersten Teil des Vortrages werden zunächst neue elementanalytische Methoden zum Nachweis von metallbasierten Nanopartikeln in Umweltmatrizes auf Basis der AF4/ICP-SFMS sowie stabilen Isotopenlabeln am Beispiel von Eisennanopartikeln vorgestellt. Im zweiten Teil wird eine neue elementanalytische Methode als komplementäre Technik zur ökotoxikologischen Bewertung von (Schad-)Stoffen vorgestellt. Die neue Methode basiert auf der on-line Kopplung von HPLC mit der single-cell-ICP-(ToF)-MS (sc-ICP-(ToF)-MS) [1, 3-5]. Hierüber konnten wir erfolgreich die automatisierte Multielementanalytik einzelner Diatomeen realisieren und zur Analyse von mit Metallen inkubierten Diatomeen (cyclotella meneghiniana) einsetzen. Wir konnten zeigen, dass die sc-ICP-ToF-MS zukünftig eine leistungsstarke, komplementäre Technik in der aquatischen Ökotoxikologie zum z.B. Test von Metallen und Nanomaterialien darstellt. T2 - GDCh Wissenschaftsforum Chemie CY - Aachen, Germany DA - 17.09.2019 KW - ICP-MS KW - Nanomaterialien KW - Single particle-ICP-ToF-MS KW - Single cell-ICP-ToF-MS PY - 2019 AN - OPUS4-49743 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Von der Au, M. A1 - Schwinn, M. A1 - Borovinskaya, O. A1 - Büchel, C. A1 - Kuhlmeier, K. A1 - Wichmann, K. A1 - Tremel, W. T1 - An automated single algae-ICP-ToF-MS Approach for the Investigation of Metal Uptake in Diatoms N2 - Entwicklung neuer ökotoxikologischer Bewertungsmethoden auf der Basis der automatisierten single cell-ICP-ToF-MS T2 - CANAS CY - Freiberg, Germany DA - 23.09.2019 KW - Automated single cell-ICP-ToF-MS KW - Diatoms KW - Ecotoxicological Assessment PY - 2019 AN - OPUS4-49744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Von der Au, M. A1 - Ley, P. A1 - Metzger, M. A1 - Sturm, M. T1 - HR-CS-GFMAS als leistungsstarkes Werkzeug zur Analyse von organisch gebundenem Fluor (EOF) in Oberflächengewässern N2 - Entwicklung einer off-line SPE HR-CS-GFMAS basierten Methode zur Analyse von extrahierbar organisch gebundenem Fluor (EOF) in Oberflächengewässern T2 - Analytik Jena Forum CY - Berlin, Germany DA - 24.10.2019 KW - HR-CS-GFMAS KW - Extrahierbar organisch gebundenes Fluor (EOF) KW - Oberflächengewässer PY - 2019 AN - OPUS4-49745 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Faßbender, Sebastian A1 - Rodiouchkina, K. A1 - Vanhaecke, F. A1 - Ley, P. A1 - Metzger, M. A1 - Von der Au, M. A1 - Sturm, M. A1 - Langhammer, N. A1 - Borovinskaya, O. A1 - Büchel, C. A1 - Wichmann, K. A1 - Tremel, W. T1 - New icp-(Tof)-MS based Methods for Material- and Environmental Analysis N2 - Entwicklung von ICP-(ToF)-MS basierten Methoden für die Spezies und Einzelorganismen und -Partikelanalytik an der Schnittstelle Material-Umwelt T2 - Analytisch Chemisches Kolloquium Uni Duisburg-Essen CY - Essen, Germany DA - 04.11.2019 KW - CE-ICP-MS KW - single cell-ICP-ToF-MS KW - single particle-ICP-ToF-MS KW - Speciation analysis PY - 2019 AN - OPUS4-49747 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Von der Au, M. A1 - Borovinskaya, O. A1 - Flamigni, L. A1 - Kuhlmeier, K. A1 - Büchel, C. T1 - An automated single algae-ICP-ToF-MS approach for the Investigation of Metal Uptake in Diatoms N2 - Entwicklung einer automatisierten single cell-ICP-ToF-MS Methode zur Analyse von metallexponierten Diatomen. T2 - CANAS CY - Freiberg, Germany DA - 23.09.2019 KW - Single cell-ICP-ToF-MS KW - Multivariate Datenauswertung KW - Diatom PY - 2019 AN - OPUS4-49748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Von der Au, M. A1 - Borovinskaya, O. A1 - Büchel, C. A1 - Meermann, Björn T1 - Der Fingerabdruck der Kieselalge N2 - Elementanalytische Verfahren werden heute zu mehr eingesetzt als bloß zur Bestimmung von Metallgesamtgehalten in diversen Probenmatrizes. Sie stellen heute ein wichtiges Werkzeug zur Beantwortung lebenswissenschaftlicher Fragen aus Umwelt, Medizin und Biologie dar. In der vorliegenden Arbeit kommt die single-cell-ICP-Flugzeitmassenspektrometrie (single-cell-ICP-TOF-MS) zur Multielementanalytik in einzelnen Kieselalgen (Diatomeen) zum Einsatz und wird zukünftig ein wichtiges Werkzeug z.B. bei der Beantwortung ökotoxikologischer Fragestellung sein. KW - Diatomeenanalytik KW - Single cell-ICP-ToF-MS KW - Multielementanalytik in kurzen transienten Signalen PY - 2019 UR - https://q-more.chemie.de/q-more-artikel/299/der-fingerabdruck-der-kieselalge.html SP - 1 EP - 3 PB - LUMITOS AN - OPUS4-49749 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Von der Au, M. A1 - Meermann, Björn T1 - Screening von Organofluorverbindungen im Oberflächenwasser N2 - Organofluorverbindungen kommen in vielen Bereichen zum Einsatz und gelangen in die aquatische Umwelt. Die Belastungssituation der Gewässer ist bisher wenig untersucht – hier kommt die HR-CS GF MAS als leistungsstarkes Screeningtool zum Einsatz. KW - HR-CS-GFMAS KW - Extrahierbar organisch gebundenes Fluor (EOF) KW - Oberflächengewässer PY - 2019 UR - https://analytik.news/Fachartikel/Volltext/bam5.pdf SP - 1 EP - 3 PB - Dr. Beyer Internet-Beratung AN - OPUS4-49750 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lardy-Fontan, S. A1 - Piechotta, Christian A1 - Heath, E. A1 - Perkola, N. A1 - Balzamo, S. A1 - Cotman, M. A1 - Gökcen, T. A1 - Gardia-Parège, C. A1 - Budzinski, H. A1 - Lalère, B. T1 - A project to deliver reliable measurements of estrogens 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 (17aE2) and estriol (E3) will be included to demonstrate the reliability of the developed methods - Mass Spectrometry based method and effect-based methods (EBM) - 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 EBM will be deeply investigated in order to improve their rationale use and their support in water quality assessment. T2 - Eurachem Workshop - Uncertainty from sampling and analysis for accredited laboratories CY - Berlin, Germany DA - 19.11.2019 KW - MS based method KW - Estrogens KW - Reliable measurements KW - Comparability KW - Effect based Method PY - 2019 AN - OPUS4-49738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lardy-Fontan, S. A1 - Piechotta, Christian A1 - Heath, E. A1 - Perkola, N. A1 - Balzamo, S. A1 - Cotman, M. A1 - Gökcen, T. A1 - Gardia-Parège, C. A1 - Budzinski, H. A1 - Lalère, B. T1 - A project to deliver reliable measurements of estrogens 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 (17aE2) and estriol (E3) will be included to demonstrate the reliability of the developed methods - Mass Spectrometry based method and effect-based methods (EBM) - 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 EBM will be deeply investigated in order to improve their rationale use and their support in water quality assessment. T2 - ICRAPHE - Second International Conference on Risk Assessment of Pharmaceuticals in the Environment CY - Barcelona, Spanien DA - 28.11.2019 KW - Estrogens KW - Effect based Method KW - Comparability KW - Reliable measurements KW - MS based method PY - 2019 AN - OPUS4-49739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Kick-off meeting “18NRM01-EDC-WFD” 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 (17aE2) and estriol (E3) will be included to demonstrate the reliability of the developed methods - Mass Spectrometry based method and effect-based methods (EBM) - 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 EBM will be deeply investigated in order to improve their rationale use and their support in water quality assessment. T2 - EMPIR Kick-off meeting EDC-WFD CY - Paris, France DA - 07.10.2019 KW - Estrogens KW - Reliable measurements KW - Effect based Method KW - Comparability KW - MS based method PY - 2019 AN - OPUS4-49741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meermann, Björn A1 - Faßbender, Sebastian T1 - Antifoulingmittel im Wasser N2 - Für das Biozid Zink-Pyrithion, das in Schiffsanstrichen weit verbreitet ist, fehlten bisher die analytischen Methoden, um den Komplex und seine Abbauprodukte in der Umwelt nachzuweisen. Kapillarelektrophorese, gekoppelt mit komplementärer Massenspektrometrie könnte dieses Problem lösen. KW - Antifouling-Biozide KW - Kapillarelektrophorese-Massenspektrometrie KW - Komplementäre Massenspektrometrie KW - Umwelt-Speziation PY - 2019 DO - https://doi.org/10.1002/nadc.20194088793 SN - 1439-9598 SN - 1868-0054 VL - 67 IS - 12 SP - 56 EP - 58 PB - Wiley-VCH CY - Weinheim AN - OPUS4-49789 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Goren, A.C. A1 - Gokcen, T. A1 - Gunduz, S. A1 - Koch, Matthias A1 - Kaloulides, E. A1 - Giannikopoulou, P. A1 - Wai-Tong, G.T. A1 - Chan, A. T1 - Report on key comparison CCQM-K138: determination of aflatoxins (AFB(1), AFB(2), AFG(1), AFG(2) and total AFs) in dried fig N2 - The presence of any aflatoxin contamination in exported figs needs to be monitored and measured through reliable and traceable methods, which require pure and matrix certified reference materials. On the other hand, certified reference materials (CRM) for determination of aflatoxins in dried fig are not yet available. Moreover, there is a lack of CRMs to be used in routine testing laboratories for method validation and quality control. The routine testing laboratories, participating in commercial proficiency testing (PT) programs, use the results available from consensus values to evaluate the performance of the participating laboratories, rather than metrologically traceable assigned values. This study initially proposed as a key comparison and presented at the EURAMET TC-MC SCOA meeting in Malta in 2015 and subsequently at the CCQM OAWG meeting in April 2015, proposes a CRM candidate for determination of levels of aflatoxins B1, B2, G1, G2 and their total in dried. Evidence of successful participation in formal, relevant international comparisons are needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). In total nine NMI/DI participated in the Track C Key Comparison CCQM-K138 Determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and Total AFs) in Dried Fig. Participants were requested to evaluate the mass fractions expressed in ng/g units, of aflatoxins B1, B2, G1, G2 and total aflatoxin in a dried food matrix, dried fig. The CCQM-K138 results for the determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and total AFs) are ranging from 5.17 to 7.27 ng/g with an %RSD of 10.47 for AFB1, ranging from 0.60 to 0.871 ng/g with an %RSD of 11.69 for AFB2, ranging from 1.98 to 2.6 ng/g with an %RSD of 10.36 for AFG1, ranging from 0.06 to 0.32 ng/g with an %RSD of 35.6 for AFG2, and ranging from 8.29 to 10.31 ng/g with an %RSD of 7.69 for Total AFs. All participants based their analyses on LC-MS/MS, HPLC-FLD, HR-LC/MS, and IDMS. Brief descriptions of the analytical methods used by the participants, including sample preparation, analytical technique, calibrants, and quantification approach are summarized in Appendix F. Linear Pool was used to assign the Key Comparison Reference Values (KCRVs) for B1, B2, G1, G2 and total aflatoxins. Due to the traceability requirements for the calibrants not being met, results of KEBS, INTI, VNIIM and BAM were excluded from KCRV determination. Successful participation in CCQM-K138 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having high polarity (pKow > -2), in mass fraction range from 0.05 ng/g to 500 ng/g in dried food matrices. KW - Aflatoxins KW - Mycotoxins KW - Dried fig KW - Food contaminants PY - 2019 DO - https://doi.org/10.1088/0026-1394/56/1A/08008 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08008-1 EP - 08008-106 PB - IOP CY - Bristol AN - OPUS4-50326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tvrdonova, M. A1 - Vlcnovska, M. A1 - Pompeiano Vanickova, L. A1 - Kanicky, V. A1 - Adam, V. A1 - Ascher, Lena A1 - Jakubowski, Norbert A1 - Vaculovicova, M. A1 - Vaculovic, T. T1 - Gold nanoparticles as labels for immunochemical analysis using laser ablation inductively coupled plasma mass spectrometry N2 - In this paper, we describe the labelling of antibodies by gold nanoparticles (AuNPs) with diameters of 10 and 60 nm with detection by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Additionally, the AuNPs labelling strategy is compared with commercially available labelling reagents based on MeCAT (metal coded affinity tagging). Proof of principle experiments based on dot blot experiments were performed. The two labelling methods investigated were compared by sensitivity and limit of detection (LOD). The absolute LODs achieved were in the range of tens of picograms for AuNP labelling compared to a few hundred picograms by the MeCAT labelling. KW - Nanoparticle KW - LA-ICP-MS KW - Labeling PY - 2019 DO - https://doi.org/10.1007/s00216-018-1300-7 SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 3 SP - 559 EP - 564 PB - Springer-Verlag GmbH CY - Berlin, Heidelberg AN - OPUS4-47093 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Weigert, Florian A1 - Frenzel, Florian A1 - Würth, Christian A1 - Hoffmann, Katrin A1 - Martynenko, Irena A1 - Dhamo, Lorena T1 - Photoluminescence Properties of Different Types of Nanocrystals at the Ensemble and Single Emitter Level N2 - Correlating the photoluminescence (PL) properties of nanomaterials like semiconductor nanocrystals (QDs) and upconversion nanocrystals (UCNPs) assessed in ensemble studies and at the single particle level is increasingly relevant for applications of these nanomaterials in the life sciences like bioimaging studies or their use as reporters in microfluidic assays. Here we present a comparison of the spectroscopic properties of ensembles and single emitters for QDs like II/VI QDs and cadmium-free AIS/ZnS QDs as well as different UCNPs. The overall goal of this study was to derive particle architectures well suited for spectroscopic and microscopic applications. T2 - BIOSSPIE CY - San Francisco, CA, USA DA - 02.02.2019 KW - Quantum yield KW - Nanomaterial KW - Photoluminescence KW - Absolute fluorometry KW - Integrating sphere spectroscopy, KW - NIR KW - IR KW - Fluorescence KW - Nanoparticle KW - Semiconductor KW - Quantum dot KW - Single particle spectroscopy KW - Surface chemistry PY - 2019 AN - OPUS4-47358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Hard X-ray spectroscopy and imaging at the BAMline and MySpot beamlines at BESSY II (Berlin, Germany) N2 - Overview of the X-ray based analytical methods conducted at the BAMline and µSpot Beamline for structure analysis. T2 - Pccr2 + AfLS conference CY - Accra, Ghana DA - 29.01.2019 KW - X-ray spectroscopy KW - Synchrotron KW - Beamline KW - Material characterization PY - 2019 AN - OPUS4-47319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Khatib, A. H. A1 - Radbruch, H. A1 - Trog, S. A1 - Neumann, B. A1 - Paul, F. A1 - Koch, A. A1 - Linscheid, M. W. A1 - Jakubowski, Norbert A1 - Schellenberger, E. T1 - Gadolinium in human brain sections and colocalization with other elements N2 - Recent recommendations by the Food and Drug Administration1 and the European Medicines Agency2 are to limit the clinical use of linear gadolinium-based contrast agents (GBCAs) due to convincing evidence of deposition in tissues. Macrocyclic GBCA continued to be considered safe, provided that patients have normal renal function. To date, given the low sensitivity of conventional MRI, there has been a debate about the signal increase following the injections of a macrocyclic GBCA. KW - Gadolinium PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471309 DO - https://doi.org/10.1212/NXI.0000000000000515 SN - 2332-7812 VL - 6 IS - 1 SP - e515, 1 EP - 3 PB - American Academy of Neurology AN - OPUS4-47130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xiao, J. A1 - Vogl, Jochen A1 - Rosner, M. A1 - Deng, L. A1 - Jin, Z. T1 - A validated analytical procedure for boron isotope analysis in plants by MC-ICP-MS N2 - Boron (B) is an essential micronutrient for plant growth. Lack of valid methods for pretreatment and measurement of δ11B in plant restrict applications of it in the biosphere. Dry ashing, one step cation exchange and micro-sublimation were combined to separate and purify boron (B) in plant tissues. The low procedure blank, high B recovery and the accurate δ11B values of the plant reference materials demonstrate that this method is suitable and valid for B pretreatment and δ11B measurement in plant samples by MC-ICP-MS. Based on this method, the δ11B in different plants (Brassica napus, Chenopodium album L, moss, lichen, and Nostoc commune) was analyzed. For Brassica napus, δ11B increased gradually from root to leaf, and then decreased to rapeseed. For the same parts, the δ11B increased from the lower parts to the higher parts. This variation may be due to the B(OH)3 transporter of NIP6;1 and the incorporation of B into the cell. The reason for lower δ11B values in shell and rapeseed compared to those in leaves presumably is to the preferred Transport of borate in the phloem. The largest δ11B fractionation between leaf and root in Brassica napus and Chenopodium album L was +24.2‰ and +26.6‰, respectively. The large variation and fractionation of δ11B within plants indicates that δ11B is a good tracer to study the B translocation mechanisms and metabolism within plants. The δ11B in Nostoc commune, lichen, and moss showed variations of -4.1‰ to +21.5‰, −9.4‰ to +7.3‰, and −18.3‰ to +11. 9‰, respectively. In the same site, δ11B in different plants ranked Nostoc commune>moss>lichen and δ11B in mosses growing in different environment ranked soil>tree>rock. Rain and soil available B are the main B sources for these plants. The δ11B in Nostoc commune, lichen, and moss may be a useful tracer to study the atmospheric B input. In the future, plants culture experiments under certain environments and studies from molecular level are necessary to decipher the variation of δ11B and fractionation mechanisms within plants. KW - Boron isotope KW - Isotopic fractionation KW - Micro-sublimation KW - Plant tissue KW - MC-ICP-MS PY - 2019 DO - https://doi.org/10.1016/j.talanta.2018.12.087 SN - 0039-9140 SN - 1873-3573 VL - 196 SP - 389 EP - 394 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-47160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471430 DO - https://doi.org/10.1088/0026-1394/56/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Sander, L. C. A1 - Wise, S. A. A1 - Philipp, Rosemarie A1 - Hein, Sebastian A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Chan, P. A1 - Lee, H. A1 - Tang, H. A1 - Tang, P. A1 - Yip, Y. A1 - Lu, T. A1 - Cheow, P. S. A1 - Teo, T. L. A1 - Sega, M. A1 - Rolle, F. A1 - Baek, S. A1 - Kim, B. A1 - Lee, S. A1 - Cabillic, J. A1 - Fallot, C. A1 - Hua, T. A1 - Dazhou, C. A1 - Changjun, Y. A1 - Chunxin, L. A1 - Hongmei, L. A1 - Lippa, K. A1 - Itoh, N. A1 - Quinn, L. A1 - Prevoo-Franzsen, D. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. A1 - Gündüz, S. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Baldan, A. A1 - van der Hout, J. W. A1 - van der Veen, A. M. H. T1 - CCQM-K131 Low-polarity analytes in a multicomponent organic solution: Polycyclic aromatic hydrocarbons (PAHs) in acetonitrile N2 - Solutions of organic analytes of known mass fraction are typically used to calibrate the measurement processes used to determine these compounds in matrix samples. Appropriate value assignments and uncertainty calculations for calibration solutions are critical for accurate measurements. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2015 the Organic Analysis Working Group (OAWG) sponsored CCQM-K131 "Low-Polarity Analytes in a Multicomponent Organic Solution: Polycyclic Aromatic Hydrocarbons (PAHs) in Acetonitrile". Polycyclic aromatic hydrocarbons (PAHs) result from combustion sources and are ubiquitous in environmental samples. The PAH congeners, benz[a]anthracene (BaA), benzo[a]pyrene (BaP), and naphthalene (Nap) were selected as the target analytes for CCQM-K131. These targets span the volatility range of PAHs found in environmental samples and include potentially problematic chromatographic separations. Nineteen NMIs participated in CCQM-K131. The consensus summary mass fractions for the three PAHs are in the range of (5 to 25) μg/g with relative standard deviations of (2.5 to 3.5) %. Successful participation in CCQM-K131 demonstrates the following measurement capabilities in determining mass fraction of organic compounds of moderate to insignificant volatility, molar mass of 100 g/mol up to 500 g/mol, and polarity pKow < −2 in a multicomponent organic solution ranging in mass fraction from 100 ng/g to 100 μg/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, and (3) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Naphthalene (Nap) KW - Organic calibration solution KW - Polycyclic aromatic hydrocarbon (PAH) PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471442 DO - https://doi.org/10.1088/0026-1394/56/1A/08003 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08003, 1 EP - 102 PB - IOP Science AN - OPUS4-47144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trog, S. A1 - El-Khatib, Ahmed A1 - Beck, S. A1 - Makowski, M. A1 - Jakubowski, Norbert A1 - Linscheid, M. T1 - Complementarity of molecular and elemental mass spectrometric imaging of Gadovist™ in mouse tissues N2 - Drug biodistribution analyses can be considered a key issue in pharmaceutical discovery and development. Here, mass spectrometric imaging can be employed as a powerful tool to investigate distributions of drug compounds in biologically and medically relevant tissue sections. Both matrix-assisted laser desorption ionization–mass spectrometric imaging as molecular method and laser ablation inductively coupled plasma–mass spectrometric imaging as elemental detection method were applied to determine drug distributions in tissue thin sections. Several mouse organs including the heart, kidney, liver, and brain were analyzed with regard to distribution of Gadovist™, a gadolinium-based contrast agent already approved for clinical investigation. This work demonstrated the successful detection and localization of Gadovist™ in several organs. Furthermore, the results gave evidence that gadolinium-based contrast agents in general can be well analyzed by mass spectrometric imaging methods. In conclusion, the combined application of molecular and elemental mass spectrometry could complement each other and thus confirm analytical results or provide additional information. KW - Laser ablation inductively coupled plasma–mass spectrometry imaging (LA-ICP-MSI) KW - Gadolinium-based contrast agents (GBCAs) KW - Matrix-assisted laser desorption ionization–mass spectrometry imaging (MALDI-MSI) PY - 2019 DO - https://doi.org/10.1007/s00216-018-1477-9 SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 3 SP - 629 EP - 637 PB - Springer AN - OPUS4-47371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Flemig, Sabine A1 - Köllensperger, G. A1 - Rusz, M. A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - LA-ICP-MS study of Ag nanoparticle transport in a three-dimensional in vitro model N2 - We have applied laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with subcellular resolution as an elemental mass microscope to investigate the distributions of Ag nanoparticles (NP) in a 3-dimentional multicellular spheroid (MCS) model. The production of MCS has been optimized by changing the seeding cell number (500 to 40,000 cells) and the growth period (1 to 10 days). Incubations of MCS with Ag nanoparticle suspensions were performed with a concentration of 5 µg mL-1 for 24 hours. Thin-sections of the Eosin stained MCS were analysed by elemental mass microscopy using LA-ICP-MS to image distributions of 109Ag, 31P, 63Cu, 66Zn and 79Br. A calibration using NP suspensions was applied to convert the measured Ag intensity into the number of particles being present in each measurement pixel. The numbers of NP determined ranged from 30 up to 4,000 particles in an enrichment zone. The particle distribution was clearly correlated to 31P, 66Zn and 79Br and was localized in an outer rim of proliferating cells (confirmed by DAPI) with a width of about two-single cell diameters. For the highest seeding cell number NPs were only detected in this outer rim, whereas small molecules as for instance 79Br and 109Ag ions were detected in the core of the MCS as well. Aniline blue staining demonstrated that this outer rim was rich in collagen structures in which fibroblast cells were embedded and a thin-membrane was visible which separated the core from the biological active cell layer functioning as biological barriers for NP transport. In this presentation, we will show the possibility using this 3-dimensional model for toxicological and medical applications. T2 - European Winter Conference on Plasma Spectrochemistry EWCPS-2019 CY - Pau, France DA - 03.02.2019 KW - Laser ablation KW - ICP-MS KW - Nanoparticles KW - Cell KW - Multicellular spheroid PY - 2019 AN - OPUS4-47374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, R. A1 - Braun, Ulrike A1 - Fankhänel, J. A1 - Daum, B. A1 - Arash, B. A1 - Rolfes, R. T1 - Molecular modelling of epoxy resin crosslinking experimentally validated by near-infrared spectroscopy N2 - Reliable simulation of polymers on an atomistic length scale requires a realistic representation of the cured material. A molecular modelling method for the curing of epoxy systems is presented, which is developed with respect to efficiency while maintaining a well equilibrated system. The main criterion for bond formation is the distance between reactive groups and no specific reaction probability is prescribed. The molecular modelling is studied for three different mixing ratios with respect to the curing evolution of reactive Groups and the final curing stage. For the first time, the evolution of reactive groups during the curing process predicted by the molecular modelling is validated with near-infrared spectroscopy data, showing a good agreement between simulation results and experimental measurements. With the proposed method, deeper insights into the curing mechanism of epoxy systems can be gained and it allows us to provide reliable input data for molecular Dynamics simulations of material properties. KW - Epoxy KW - NIR spectroscopy KW - Modelling PY - 2019 DO - https://doi.org/10.1016/j.commatsci.2019.01.054 SN - 0927-0256 VL - 161 SP - 223 EP - 235 PB - Elsevier AN - OPUS4-47431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klöckner, P. A1 - Reemtsma, T. A1 - Eisentraut, Paul A1 - Braun, Ulrike A1 - Ruhl, A. S. A1 - Wagner, S. T1 - Tire and road wear particles in road environment e Quantification and assessment of particle dynamics by Zn determination after density separation N2 - In this study, a method for the determination of tire and road wear particle (TRWP) contents in particulate samples from road Environment was developed. Zn was identified as the most suitable elemental marker for TRWP, due to its high concentration in tire tread and the possibility of separation from other Zn sources. The mean concentration of 21 tire samples was 8.7 ± 2.0 mg Zn/g. Before quantification in samples from road environment, TRWP were separated from the particulate matrix by density separation. Method development was conducted using shredded tread particles (TP) as a surrogate for TRWP. Recovery of TP from spiked sediment was 95 ± 17% in a concentration range of 2 - 200 mg TP/g. TP determination was not affected by other Zn containing solids or spiked Zn-salts. By adjusting the density of the separation solution to 1.9 g/cm3, more than 90% of total TRWP were separated from the sample matrix. TRWP concentrations in particulate matter collected in two road runoff treatment Systems ranged from 0.38 to 150 mg TRWP/g. Differences in quantified TRWP contents of the two Systems indicate changes in particle dynamics due to ageing and aggregation processes. The developed method allows TRWP determination in road runoff and in environments that are influenced by road traffic. The validated separation procedure can also be applied for TRWP characterization in future studies. KW - Zinc analysis KW - Microplastics KW - Tire particles PY - 2019 VL - 222 SP - 714 EP - 721 PB - Elsevier AN - OPUS4-47433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - ISO-Guide 35 in der Praxis eines RM-Herstellers N2 - Der ISO-Guide 35 beschreibt die notwendigen Schritte zur Herstellung von zertifizierten Referenzmaterialien. Anhand praktischer Beispiele wird die Umsetzung des Guide 35 in der BAM dokumentiert. T2 - DAkkS-Informationsveranstaltung - Akkreditierung von Referenzmaterialherstellern; Fachbereich Ringversuche / Referenzmaterialien CY - Berlin, Germany DA - 14.02.2019 KW - ZRM KW - ISO-Guide 35 KW - Referenzmaterial-Herstellung PY - 2019 AN - OPUS4-47395 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaimenko, I. A1 - Jaeger, C. A1 - Brenner, H. A1 - Chang-Claude, J. A1 - Hoffmeister, M. A1 - Grötzinger, C. A1 - Detjen, K. A1 - Burock, S. A1 - Schmitt, C.A. A1 - Stein, U. A1 - Lisec, Jan T1 - Non-invasive metastasis prognosis from plasma metabolites in stage II colorectal cancer patients: The DACHS study N2 - Metastasis is the main cause of death from colorectal cancer (CRC). About 20% of stage II CRC patients develop metastasis during the course of disease. We performed metabolic profiling of plasma samples from non-metastasized and metachronously metastasized stage II CRC patients to assess the potential of plasma metabolites to serve as biomarkers for stratification of stage II CRC patients according to metastasis risk. We compared the metabolic profiles of plasma samples prospectively obtained prior to metastasis formation from non-metastasized vs. metachronously metastasized stage II CRC patients of the German population-based case–control multicenter DACHS study retrospectively. Plasma samples were analyzed from stage II CRC patients for whom follow-up data including the information on metachronous metastasis were available. To identify metabolites distinguishing non-metastasized from metachronously metastasized stage II CRC patients robust supervised classifications using decision trees and support vector machines were performed and verified by 10-fold cross-validation, by nested cross-validation and by traditional validation using training and test sets. We found that metabolic profiles distinguish non-metastasized from metachronously metastasized stage II CRC patients. Classification models from decision trees and support vector machines with 10-fold cross-validation gave average accuracy of 0.75 (sensitivity 0.79, specificity 0.7) and 0.82 (sensitivity 0.85, specificity 0.77), respectively, correctly predicting metachronous metastasis in stage II CRC patients. Taken together, plasma metabolic profiles distinguished non-metastasized and metachronously metastasized stage II CRC patients. The classification models consisting of few metabolites stratify non-invasively stage II CRC patients according to their risk for metachronous metastasis. KW - Mass-Spectrometry KW - Cancer PY - 2019 DO - https://doi.org/10.1002/ijc.32076 SN - 1097-0215 VL - 145 IS - 1 SP - 221 EP - 231 PB - Wiley AN - OPUS4-47465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Keller, Julia A1 - Lörchner, Dominique A1 - Mekonnen, Tessema F. A1 - Koch, Matthias T1 - Transformation products of organic contaminants and residues - Overview of current simulation methods N2 - The formation of transformation products (TPs) from contaminants and residues is becoming an increasing focus of scientific community. All organic compounds can form different TPs, thus demonstrating the complexity and interdisciplinarity of this topic. The properties of TPs could stand in relation to the unchanged substance or be more harmful and persistent. To get important information about the generated TPs, methods are needed to simulate natural and manmade transformation processes. Current tools are based on metabolism studies, photochemical methods, electrochemical methods, and Fenton's reagent. Finally, most transformation processes are based on redox reactions. This review aims to compare these methods for structurally different compounds. The groups of pesticides, pharmaceuticals, brominated flame retardants, and mycotoxins were selected as important residues/contaminants relating to their worldwide occurrence and impact to health, food, and environmental safety issues. Thus, there is an increasing need for investigation of transformation processes and identification of TPs by fast and reliable methods. KW - Transformation product KW - Electrochemistry KW - Photochemistry KW - Fenton’s reagent PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474108 DO - https://doi.org/10.3390/molecules24040753 SN - 1420-3049 VL - 24 IS - 4 SP - 753, 1 EP - 23 PB - MDPI CY - Basel AN - OPUS4-47410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - About Standardization and Analytics of Microplastics N2 - Presentation about national and international standardization of microplastic analysis, as well as the project RUSEKU T2 - Industrievereinigung Chemiefaser e.V. CY - Frankfurt, Germany DA - 26.02.2019 KW - Standardisation KW - Microplastic KW - Analysis PY - 2019 AN - OPUS4-47577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik in der Umwelt und im Trinkwasser: Einordnung der Relevanz und der Methodik N2 - Überblick zur Thematik Mikroplastik mit speziellem Fokus auf Trinkwasser T2 - 20. Jahrestagung Trinkwasserringversuche Nordrhein-Westfalen – Niedersachsen CY - Osnabrück, Germany DA - 06.03.2019 KW - Trinkwasser KW - Umwelt KW - Mikroplastik PY - 2019 AN - OPUS4-47578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Müller, Axel A1 - Grathwohl, P. A1 - Vogler, M. A1 - Scholz, K. T1 - Plastik im Boden, Aktueller Forschungsstand N2 - Der Vortrag gibt einen Überblick über ein laufendes Vorhaben zum Thema Mikroplastik in Böden. T2 - NUA-Veranstaltung "Plastik in Natur und Umwelt" CY - Münster, Germany DA - 08.03.2019 KW - Mikroplastik KW - Böden KW - Analytik PY - 2019 AN - OPUS4-47579 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Bannick, C. G. T1 - Harmonisierung von Untersuchungsverfahren für (Mikro-)Plastik in der Umwelt N2 - Im Rahmen der Thematik "Recycling von Kunststoffen" wird die Thematik "Mikroplastik" vorgestellt T2 - Berliner Recycling- und Rohstoffkonferenz CY - Berlin, Germany DA - 11.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47582 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Eisentraut, Paul A1 - Dümichen, E. T1 - Analytik von Mikroplastik mittels Thermoextraktion Desorption Gas Chromatographie Massen Spektrometrie (TED-GC-MS): Nun auch die Luft? N2 - Der Vortrag gibt eine Überblick über die Messung von Mikroplastik mittels TED-GC-MS mit speziellem Fokus auf Luftgetragene Partikel T2 - Odour and Emissions of Plastic Materials CY - Kassel, Germany DA - 19.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47583 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lisec, Jan T1 - Mass-Spectrometry to conduct metabolomics experiments N2 - The presentation gives an overview in MS-Technology, the process of metabolomics experiments and the use in Fluxomics studies as a particular example. T2 - Seminar CY - Max Delbrück Center for Molecular Medicine, Germany DA - 21.03.2019 KW - Mass-Spectrometry KW - Fluxomics PY - 2019 AN - OPUS4-47663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotthoff, Lisa A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - Investigation of the veterinary drug monensin: Simulation and identification of transformation products N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for health, food and environmental matters. Monensin (MON) is an ionophore antibiotic widely used to cure and prevent coccidiosis by chicken especially in broiler farming. Residues are not only found in food products (chicken and eggs) but also in the environment (manure, soil or water). Several transformation processes can alter the parent compound MON, ranging from biotransformation in living organism to biotic/abiotic and microbial processes in environmental matters. The main objective of this work was to investigate the potential of electrochemistry (EC) to simulate oxidative transformation processes and to predict TPs of MON. An electrochemical reactor was used consisting of a flow-through cell with a glassy carbon working electrode. Derived TPs were analyzed by online coupling of EC and high-resolution mass spectrometry (HRMS) and LC-HRMS offline measurements. Among the generated TPs already known as well as unknown TPs of MON could be found. Additionally, MON was subjected also to other transformation methods such as Fenton reaction, photochemical and hydrolysis experiments as well as metabolism tests with microsomes. As a result, different targeted and suspected TPs could be identified by analysis with LC-HRMS. An overview of detected/identified TPs from this study will be presented in comparison to literature known metabolites and TPs. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Transformation Products KW - Electrochemistry KW - High-resolution MS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476813 AN - OPUS4-47681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geilert, S. A1 - Varekamp, J. C. A1 - Vogl, Jochen A1 - Frank, M. A1 - Cauley, C. A1 - Van Bergen, M. T1 - Si isotope fractionation during BIF formation – inferences from a modern Archean ocean analogue N2 - Silica-rich sedimentary rocks like cherts and BIFS, typical for the Archean, have been used to reconstruct temperatures and other properties of the early oceans through the study of their Si isotope variations. Precambrian cherts and BIFS span a δ30Si range of ~7‰, with BIFs being about 2‰ lower in δ30Si than cherts. These lower δ30Si signatures have been attributed to represent contributions from different input sources such as hydrothermal fluids, variable continental weathering regimes or sorption onto Fe oxides/hydroxides [e.g. 2 and references therein]. In this study, fluids and BIF-like sediments have been investigated for their Si isotope compositions in Paulina Lake (PL), a hydrothermally-influenced crater lake in the Newberry Caldera, Oregon, USA. PL lake sediments are rich in silica (~65wt% SiO2) and are composed of up to 22.5wt% Fe2O3, which is comparable to Archean BIFs and thus serve as a modern Archean ocean analogue. We compared our analyses with East Lake (EL), the twin Newberry crater lake without hydrothermal input. Dissolved Si in EL has an average δ30Si signature of +1.55±0.16‰ (1sd) and sediments an average δ30Si signature of +0.18±0.28‰ (1sd). Dissolved Si in PL has an average δ30Si signature of +2.02±0.15‰ (1sd), whereas the sediments show a large range in δ30Si values between +0.59‰ and -1.24‰. PL sediments show a trend towards more negative δ30Si with increasing Fe2O3 contents. The magnitude of Si isotope fractionation thus appears to depend on the presence of Fe. This fractionation induced by interaction with Fe precipitation is defined here as the offset in δ30Si between PL and EL sediments at comparable depths (Δ30SiPL-EL). The resulting Δ30SiPL-EL values range between +0.69 and -1.42‰ and increase with increasing Fe2O3 content in the sediments. Our results are the first to quantify the magnitude of Fe-induced δ30Si fractionation observed in a natural analogue of the Archean ocean and can explain the lighter δ30Si signatures found in BIFs. T2 - Fourth General Meeting of the SPP 1833 “Building a Habitable Earth” CY - Cologne, Germany DA - 27.03.2019 KW - Archean ocean KW - Si isotope fractionation KW - Delta values PY - 2019 AN - OPUS4-47711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Schaupp, Thomas A1 - Münster, C. A1 - Mente, Tobias A1 - Kannengießer, Thomas A1 - Böllinghaus, Thomas T1 - Hydrogen determination in welded specimens by carrier gas hot extraction - a review on the main parameters and their effects on hydrogen measurement N2 - Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in weld joints using a thermal conductivity detector (TCD) for hydrogen measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries (ISO 3690 type B and small cylindrical samples), and factors that additionally influence hydrogen determination. They are namely specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PI-furnace controller, as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up to the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by Evaluation of the recorded data. Generally, independent temperature measurement with dummy specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA). KW - Hydrogen KW - Carrier gas hot extraction KW - Experimental design KW - Thermal conductivity device PY - 2019 DO - https://doi.org/10.1007/s40194-018-0664-9 SN - 0043-2288 VL - 63 IS - 2 SP - 511 EP - 526 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen A1 - Lauer, F. A1 - Seifert, S. A1 - Diehn, S. A1 - Kneipp, Janina T1 - MALDI-TOF MS und MALDI-MSI zur Identifikation und Klassifizierung von Pollen N2 - Es werden die letzten Ergebnisse präsentiert, die es ermöglichen, einzelne Pollenkörner unterschiedlicher Arten in Mischungen mittels MALDI-TOF Massenspektrometrie bzw. MALDI-TOF Imaging zu messen und unter Zuhilfenahme multivariater Auswertemethoden zu klassifizieren. T2 - 24. Bruker MALDI Anwendertreffen CY - Leipzig, Germany DA - 18.02.2019 KW - MALDI-TOF Massenspektrometrie KW - Pollenkörner KW - Klassifizierung KW - MALDI Imaging KW - Multivariate Analyse PY - 2019 AN - OPUS4-47441 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Sternbaek, L. A1 - Kimani, Martha Wamaitha A1 - Gawlitza, Kornelia A1 - Janicke, B. A1 - Alm, K. A1 - Gjörloff-Wingren, A. T1 - Digital Holographic Cytometry: Macrophage Uptake of Nanoprobes N2 - Digital holographic cytometry (DHC) is a state-of-the-art quantitative Phase imaging (QPI) method that permits time-lapse imaging of cells without induced cellular toxicity. DHC platforms equipped with semi-automated image segmentation and analysis software packages for assessing cell behavior are commercially available. In this study we investigate the possible uptake of nanoprobes in macrophages in vitro over time. KW - Macrophages KW - MIPs KW - Holographic microscopy KW - Sialic acid PY - 2019 VL - 21 SP - 21 EP - 23 PB - Wiley CY - Imaging and Microscopy AN - OPUS4-47793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt (RUSEKU) N2 - Im Rahmen des Statuskonferenz der BMBF Fördermassnahme wurde über den Projektfortschritt berichtet. T2 - Statusfonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Sedimenttaionskasten KW - Probenahme KW - Mikroplastik KW - TED-GC-MS PY - 2019 AN - OPUS4-47796 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik Analytik: Probennahme, Probenaufbereitung, Detektionsverfahren N2 - Das Diskussionspapier zur Mikroplastik Analytik wurde vorgestellt. Es entstand im Rahmen des Querschnitthemas 1 des BMBF Forschungsschwerpunktes Plastik in der Umwelt. T2 - Statuskonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Harmonisierung KW - Mikroplastik KW - Probenahme KW - Detektion KW - Aufbereitung PY - 2019 AN - OPUS4-47797 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -