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 - 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 - CONF A1 - Abad Andrade, Carlos Enrique T1 - Tanz der Moleküle: Herkunftsbestimmung mittels optischer Spektroskopie N2 - Wie lässt sich die Herkunft von Rohstoffen, Lebensmitteln oder Umweltschadstoffen einfacher, schneller und kostengünstiger als mit bisherigen Methoden bestimmen? Die Dissertation zeigt auf, dass man das grundlegende physikalische Prinzip einer Isotopverschiebung mit in Adlershof entwickelten Optik-Instrumenten für die Herkunftsbestimmung nutzen kann. Die entwickelte Methode ermöglicht es in Zukunft den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Methoden möglich ist. Kann man das grundlegende physikalische Prinzip einer Isotopieverschiebung mit einem Optik-Instrument für die Herkunftsbestimmung nutzen? Carlos Abad hat eine wegweisende Methode entwickelt, die es in Zukunft ermöglicht den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Techniken möglich ist. T2 - Dissertationspreis Adlershof 2019 CY - Berlin, Germany DA - 12.02.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie KW - Coltan PY - 2020 AN - OPUS4-51993 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Immunomagnetic ochratoxin a assay with electrochemical 3,3′,5,5′ tetramethylbenzidine detection N2 - The demand for miniaturized analytical devices monitoring important parameters in the food and medical industry has increased strongly in the past decades. With fast progress, smart technologies are finding their way into our everyday life. For the future, it is, therefore, a major goal to also link analytical methods with smart technologies to create user-friendly on-site devices. In food industry the monitoring of harmful substances such as dioxins, heavy metals or mycotoxins plays a key role, since the European Commission prescribes legal limits for various food products and beverages[1]. Therefore, companies often have their own laboratories and trained personnel. For one of the most abundant and toxic mycotoxins, Ochratoxin A (OTA) we want to present an electrochemical detection system in which the read-out can be performed with a smartphone connected via Bluetooth to a miniaturized potentiostat. The recognition of OTA is performed with specific antibodies in a competitive assay format. Anti-OTA-antibodies were captured on magnetic beads on which the competitive binding between OTA and an OTA horseradish peroxidase (HRP) tracer was performed. To quantify OTA, the enzymatic reaction of the tracer with 3,3′,5,5′-tetramethylbenzidine (TMB) and H2O2 is employed. Oxidized TMB, which is enzymatically produced by the reduction of H2O2, is quantified by amperometry with screen-printed electrodes in a custom-made flow system. The results of the electrochemical detection method are in good correlation with the photometric detection of TMB. To demonstrate the applicability, we tested our system with OTA-spiked beer and performed the measurement via smartphone. T2 - 23rd JCF-Frühjahrssymposium 2021 CY - Online meeting DA - 29.03.2021 KW - Ochratoxin A KW - Cyclic voltammetry KW - Amperometry KW - Electrochemistry PY - 2021 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-52390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von Törne, Wipert A1 - Piechotta, Christian A1 - Karnstedt, L. T1 - Einblicke in das Transformationsverhalten von Warfarin N2 - Warfarin 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 (U. S. Food and Drug Administration) 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 unter umweltrelevanten Bedingungen zu erhalten und um diese Einflüsse zu simulieren, wurde hierzu eine elektrochemische Reaktorzelle in Kopplung mit einem Massenspektrometer verwendet. So können mögliche Phase-I-Metabolite und sogenannte „oxidation products“ vorausgesagt werden. Hinsichtlich des Verhaltens während der Wasseraufbereitung in Kläranlagen wurden technisch relevante Prozesse wie Chlorung, UV-Bestrahlung und Ozonung in Modellen simuliert, um hier potenzielle Abbauwege und -prozesse aufzuklären. Gebildete Transformationsprodukte wurden daher mittels unterschiedlicher chromatografischer Verfahren getrennt und massenspektrometrisch identifiziert, charakterisiert und verglichen. T2 - 49. Jahrestagung der GUS CY - Online meeting DA - 24.03.2021 KW - Warfarin KW - Transformationsprodukte PY - 2021 AN - OPUS4-52354 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Molecularly Imprinted Polymers with Integrated Fluorescence as Versatile Biomimetic Sensing Matrices N2 - Molecularly imprinted polymers (MIPs) are an established, versatile and high-performance matrix for the selective separation or enrichment of (bio)chemical species, especially small molecules of biochemical or environmental relevance. MIPs are prepared through the polymerization of a mixture of functional monomers and cross-linkers in the presence of the template with subsequent extraction of the latter. Conceptionally, this process can be seen as mimicking in a strongly accelerated, though single-step manner a biological process such as antibody formation. Because the resulting MIPs contain cavities in their matrix that are complementary in size, shape and electronic/ electrostatic or hydrogen bonding demand to the imprinted target molecule or template, these polymers are frequently termed “artificial antibodies”. Compared to natural antibodies, they are chemically and physically much more robust. Regarding sensitivity and selectivity, however, there is still a gap to bridge before MIPs can fully compete with antibodies. Another favorable aspect that distinguishes MIPs from antibodies is that they can be endowed with an explicit function, allowing the use of MIPs in applications that require more than only an efficient binder. For instance, if specifically designed and polymerizable fluorescent indicators are integrated as functional monomers into a MIP, direct fluorescence sensing can be accomplished. Because MIPs can be prepared in a variety of different formats, their combination with miniaturized or other specific analytical techniques or sensory devices is possible, especially when the transduction mode is light. This presentation will introduce basic design considerations, challenges, limitations and the potential that lies with such sensor materials with some recent examples of our group, targeting various organic oxoanions as analytes. T2 - 8th International Symposium on Bioanalysis, Biomedical Engineering and Nanotechnology CY - Changsha, Hunan, China DA - 25.05.2018 KW - Molecularly imprinted polymers KW - Fluorescence KW - Anion recognition PY - 2018 AN - OPUS4-45641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica A1 - Grunert, Bianca A1 - Jakubowski, Norbert A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Emmerling, Franziska T1 - Tagging reagents for imaging mass cytometry N2 - In der klinischen Diagnostik werden für zytometrische Messverfahren bereits eine Reihe von Reagenzien eingesetzt zur Markierung von Antikörper eingesetzt, um die Detektion von Biomarkern mittels Fluoreszenz- oder Flugzeitmassenspektrometrie zu ermöglichen. Seit kurzem ist auch eine Imaging Mass Cytometry Kombination direkt erhältlich, wodurch der Nachweis von Biomarkern in Gewebeschnitten erreicht werden kann. Dazu wird eine Kopplung von Laser Ablation und induktiv gekoppeltem Plasma Massenspektrometrie eingesetzt, wobei ähnlich der Massenzytometrie, zuvor Antikörper mit Metallen markiert, und im Anschluss mit dem Gewebeschnitt inkubiert werden. Durch die hohe Ortsauflösung können die Biomarker lokalisiert, und zukünftig vielleicht auch quantifiziert werden. Insbesondere Lanthanide eignen sich als Markierungsmetalle, da sie einen niedrigen Untergrund und chemisch ähnliches Verhalten zueinander aufweisen. Allein durch diese Elemente können bereits etwa 15 Parameter unterschieden werden, was durch isotopenreine Standards weiter gesteigert werden kann. Vom Markierungsgrad abhängig werden unterschiedlich viele Metalle am Antikörper gebunden, und beeinflussen so die Sichtbarkeit im ICP-MS. Nanopartikel könnten daher eine deutliche Steigerung der Sensitivität bewirken. GdVO4 Nanokristalle scheinen bisher sehr vielversprechend und bieten neben multiparametrischen Anwendungen auch Multimodalität. Die Synthese der Nanokristalle zeigte hohe Homogenität und Reproduzierbarkeit in Partikelgröße in der Zusammensetzung. Ein erstes Experiment mit einer Zellkultur konnte bereits die effiziente Markierung der Zellen unter Beweis stellen, wobei durch hohe Signalstärke auch subzelluläre Auflösung in der LA-ICP-MS erreicht werden konnte. T2 - ICPMS Anwendertreffen 2018 CY - Berlin, Germany DA - 03.09.2018 KW - LA-ICP-MS KW - Immuno assay KW - Bioimaging KW - Nanocrystal KW - Lanthanide KW - Metal-tag PY - 2018 AN - OPUS4-45866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Iznaguen, H. A1 - Traub, Heike A1 - Ostermann, Markus T1 - LA-ICP-MS- und RFA-Messungen für die Bestimmung von polybromierten Flammschutzmitteln (PBFSM) in Polystyrol- und Polypropylenproben N2 - To investigate the release and migration of flame retardants from polypropylene (PP) and polysytrene (PS) we use samples of with defined content of flame retardants as additives. Therefore we use HBCD in the concentration of 1% wt. resp. BDE-209 in the concentration of 0.1% wt. For the preparation of the samples granular of PP resp. PS are extruded together with the BFRs additives. Even the result of this process may lead to homogenous partition of the BFRs additives, this has to be proven before using the samples in the experimental setup for weathering studies. In accordance to the regulation of RoHS, where the use of XRF is recommended for the proof of flame retardants in electronic consumer products, we use this method as a reference to the laser ablation ICP/MS. Therefore we present the correlation of these experiments. The experimental setup for the XRF experiment is like a standard addition: in cavities, which are introduced in the sample plates subsequently, solutions of defi ned concentration of flame retardants are put in these cavities. According to the idea of standard addition, we get an information of the originating concentration of flame retardant in each sample and we can monitor the release and migration of these additives during/after the weathering experiment with high precision. Therefore to the designated plates an internal standard is added as a marker and can be analyzed after the weathering experiment. As awaited, the light exposed site, shows a deviating content in flame retardants compared to the sheltered site. N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umweltbeständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz, die jeweils mit polybromierten Flammschutzmitteln (PBFSM) versehen sind. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Auch soll mit Hilfe der RFA und der LA-ICP-MS die Abreicherung der PBFSM in den Modellmaterialien beschrieben werden. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - Umwelt 2018 CY - Münster, Germany DA - 09.09.2018 KW - PBFSM KW - RFA KW - LA-ICP-MS KW - Polypropylen KW - Polystyrol PY - 2018 AN - OPUS4-47028 LA - deu 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 - 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 - CONF A1 - Loehr, Konrad T1 - Towards single cell arraying for LA-ICP-MS N2 - Analysis of single cells via LA-ICP-MS is a technique with great potential, however manual targeting of single cells is laborious and therefore microarraying of cells looks promising. In this work, we investigate the potential of a commercial non-contact piezo dispenser arraying system (S3, Scienion AG, Berlin), equipped with a novel technology for single-cell isolation called CellenONE™ (Cellenion, Lyon). Usually if one aims to create a microarray of single cells via spotting a suitably diluted cell suspension, one will observe a Poisson-distributed cell number per spot. CellenONE™ overcomes this problem by controlling the number of cells optically in the piezo dispense capillary (PDC) via image recognition to obtain true single cell arrays. The figures of merit of the customized and optimized setup will be presented. In a proof of concept experiment we investigated the trace elemental fingerprint of THP-1 cells by LA-ICP-TOF-MS (Analyte G2, Teledyne Cetac; icpTOF, TOFWERK) and quantified two metal cell dyes, mDOTA-Ho (CheMatech, Dijon), and Ir-DNA intercalator (Fluidigm, San Francisco). For that, matrix matched calibration standards after Wang et al. were successfully prepared using the same arraying system. We believe that this novel approach opens new ways for automated quantitative single cell LA-ICP-MS. T2 - DIAGNOSTICS 8.0 CY - Berlin, Germany DA - 06.09.2018 KW - High throughput KW - Single cell KW - Laser ablation KW - ICP-MS KW - CellenONE PY - 2018 AN - OPUS4-45904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - LA-ICP-MS for the analysis of nanoparticles in cells N2 - Many current nanomaterials can serve as contrast agents in cellular or tissue imaging, drug delivery vehicles or therapeutics, whereas others can cause toxic effects. In order to evaluate nano-bio interactions, the number of nanoparticles (NPs) inside cells as well as their localisation within cellular substructures is of particular interest. The cellular uptake depends on the primary characteristics of the NPs (e.g. size, shape, surface coating) and on the cell type. Laser ablation inductively coupled plasma mass spectrometry (LA‑ICP‑MS) is more and more used to study the NP pathway from uptake, via intracellular processing up to cell division. High-spatial resolution laser ablation at single cell level is achieved using novel low-dispersion LA chambers and by careful optimisation of laser energy, ablation frequency and scan speed at small laser spot sizes down to 1 µm. Different examples from BAM, Division 1.1 and cooperation partners using LA-ICP-MS to localize and quantify metal-containing nanoparticles are shown. The results demonstrate the potential of LA-ICP-MS providing insight into NP uptake, intracellular distribution and cell-to-cell variation. T2 - 13. Symposium "Massensprektrometrische Verfahren der Elementspurenanalyse" + 26. ICP-MS Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Laser ablation KW - Cells KW - Nanoparticles KW - Imaging PY - 2018 AN - OPUS4-46440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raysyan, Anna A1 - Raysyan, Anna T1 - Development of dipstick immunoassays for environmental and diagnostic applications missions from plastic materials N2 - Development of dipstick immunoassays for environmental analysis and integration the technology for diagnostic applications missions. T2 - Arbeitskreistreffen Immunoassays CY - Hennigsdorf, Germany DA - 26.11.2018 KW - Environmental analysis KW - LFIA KW - BPA KW - DCF PY - 2018 AN - OPUS4-46801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raysyan, Anna T1 - Breaking the wall of complicated laboratory methods N2 - How intricate lab methods make it to the lay(wo)men’s hand. T2 - Falling Walls Lab Adlershof CY - Berlin, Germany DA - 28.09.2018 KW - Easy-use device PY - 2018 AN - OPUS4-46755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Völker, Tobias A1 - Kazakov, Alexander Ya. T1 - Improved algorithm for calibration-free laser induced breakdown spectroscopy N2 - An improved algorithm for calibration-free laser induced breakdown spectroscopy (CF LIBS) will be presented which includes several novel features in comparison with previously proposed similar algorithms. In particular, it allows using spectral lines with arbitrary optical thickness for the construction of Saha-Boltzmann plots, retrieves the absorption path length (plasma diameter) directly from a spectrum, replaces the Lorentzian line profile function by the Voigt function, and allows for self-absorption correction using pre-calculated and tabulated data rather than approximating functions. The tabulated data embody the solutions of the radiative transfer equation for numerous combinations of optical thicknesses and line widths. The algorithm is thoroughly verified using synthetic spectra. T2 - LIBS 2018 at SciX 2018 CY - Atlanta, GA, USA DA - 21.10.2018 KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2018 AN - OPUS4-46930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Nirmalanthan-Budau, Nithiya A1 - Moser, Marko A1 - Roloff, Alexander A1 - Moldenhauer, Daniel T1 - Quantification of Surface Groups on Nanomaterials with Simple Optical Methods N2 - Surface functionalization of nanomaterials is nowadays at the core of many applications of functional materials in the life and material sciences. Examples range from membranes and microarrays over bead-based assays, and next generation sequencing to nanometer-sized optical reporters, nanosensors, and magnetic and optical contrast agents. Typical function-nalization steps include silanization and grafting reactions with reactive monomers to introduce functional groups like amino or carboxylic acid groups or the attachment of ligands like polyethylene glycol (PEG) molecules and biomolecules. [1-3] This enables to tune e.g., dis-persibility, hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunctionalization efficiencies, and enhance blood circulation times and allows for the use of nanomaterials as reporters in assays or the design of targeted probes for bioimaging. At the core of all functionalization strategies are reliable and validated methods for surface group and ligand quantification that can be preferably performed with routine laboratory instrumentation, require only small amounts of substances, and are suitable for many different types of nanomaterials. [3] There is meanwhile a considerable need to make these methods traceable. We present here versatile and simple concepts for the quantification of common functional groups, ligands, and biomolecules on different types of organic and inorganic nanomaterials, using conventional and newly developed cleavable and multimodal reporters, that can be detected with optical spectroscopy. [4-7] These reporters are chosen to enable method validation with the aid of method comparisons and mass balances. Also, strategies how to make these simple assays traceable to SI units using quantitative nuclear resonance spectroscopy (qNMR) and X-ray photoelectron spectroscopy (XPS) are derived. T2 - JRC-NIST Workshop CY - Ispra, Italy DA - 04.12.2018 KW - Nanoparticle KW - Nanocrystal KW - Absolute fluorometry KW - Fluorescence KW - Surface chemistry KW - Assay KW - Cleavable probe KW - Conductometry KW - Quantification KW - Functional group PY - 2018 AN - OPUS4-46950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röthke, A. A1 - Richter, Silke A1 - Görlitz, V. A1 - Pape, C. A1 - Schulz, U. A1 - Jährling, R. A1 - Meinhardt, R. A1 - Koenig, M. A1 - Becker, D. A1 - Charoud-Got, J. A1 - Weber, M. A1 - Rienitz, O. T1 - As good as or even better than ID-ICP-MS? High accuracy ICP OES determination of 1 g/kg mercury solutions N2 - To establish the SI traceability of the element content w(Hg) of a gravimetrically prepared 1 g/kg mercury solution, the latter was compared to a primary reference solution by means of high accuracy inductively coupled plasma optical emission spectrometry (ICP OES) measurements. For this purpose, the ICP OES bracketing method previously described [1] was improved to yield a relative expanded uncertainty of the mercury element content of Urel(w(Hg)) = 0.5 % (with k = 2) associated with the comparison of two monoelemental solutions. In case of mercury, such a small uncertainty was achieved for the first time. Before, in general, such small uncertainties were only reported applying isotope dilution methods performed with MC-ICP-MS. However, for mercury solutions at this concentration range, several dilution steps are necessary to prepare the samples for ID-MC-ICP-MS. The sum of the uncertainty contributions stemming from the dilution steps, as well as the intrinsic difficulties of measuring mercury at low concentrations, result in an overall uncertainty of the ICP-MS measurements, which is comparable to or even larger than those, achieved with the ICP OES method applied. We will present details of the sample preparation as well as of the dedicated ICP OES measurement approach, which were crucial to achieve such a small measurement uncertainty. The newly developed method was successfully applied in the context of the development and production of elemental solution chemical reference standards (CRS), which are distributed by the EDQM. The CRS are intended to support measurements required by the European Pharmacopoeia, which has recently incorporated a new international guideline for the control of elemental impurities in medicinal products. T2 - ICP-MS Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Traceability KW - Mercury solution PY - 2018 AN - OPUS4-46218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Zertifizierung von Referenzmaterialien an der BAM N2 - Wege zur Zertifizierung von Referenzmaterialien an der BAM werden anhand des Leitfadens und praktischer Beispiele gegeben. T2 - Schulung zur Zertifizierung von RM CY - Berlin, Germany DA - 11.04.2018 KW - Referenzmaterialien KW - Zertifizierung PY - 2018 AN - OPUS4-46221 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, V. A1 - Richter, Silke T1 - Progress at the calibration of light elements N2 - Analytical glow discharges with optical (GD-OES) and mass spectrometric (GD-MS) detection are able to obtain depth resolved information about the light elements hydrogen, carbon, nitrogen and oxygen in solid samples, where most of the other analytical techniques fail. However, the interpretation or even quantification of the measured signals is still very challenging. Problems arise due to physical effects (plasma processes such as the ‘Hydrogen effect’, the Doppler effect, self absorption or diffusion of hydrogen in the sample during sputtering) chemical effects(e.g. formation of compounds with argon or the matrix, poisoning of the sample or gettering) as well as instrumental difficulties (e.g. of the sensitivity, calibration and vacuum quality).. The GD techniques are direct solid sampling methods and require reference materials for calibration. Unfortunately the list of available certified reference materials (CRM) suited for calibration of light elements in different matrix is relatively short Therefore, sintered materials doped with the analytes H2, O2 and N2 were produced at IFW Dresden and applied as calibration standards for hydrogen, oxygen and nitrogen. Due to the high analyte concentration added, it is very likely that the real concentration agree well with the added amount of light elements in the corresponding phases. The validation of the determination of the light element concentration in the sintered samples was possible in some cases only due to the lack of suitable techniques. This fact proves the need for the development of a reliable quantification of light elements by GDS. A systematic dependence of the sputtering rate on the composition was found and can be explained by basic principles. Using mixtures of TiH2 and ZrH2 with Cu the ratio of hydrogen and Cu lines has a good correlation with the corresponding concentration ratio. The hydrogen emission yield however decreases over 0.3 m% hydrogen and finally the hydrogen intensity may even decrease. This behaviour can be explained by a very similar quenching of the hydrogen and copper intensity caused by the hydrogen effect. First experiments with GD-MS show no saturation of the hydrogen ion current and thus confirm the quenching of the emission yield in GD-OES. Sintered material for the oxygen calibration (Al2O3, CuO, Cu2O and MgO mixed with Cu, Al and Mg) confirmed the blue line shift effect at O I 130.22 nm, first time reported by Köster 2009 [1]. The effect is more pronounced at Mg than in Al and Cu, which due to line interference leads to a matrix dependent EY. This effect is negligible at O I 777.19 nm and the EY is matrix independent. Using GD-MS first promising results for the calibration of oxygen with these sintered samples could be obtained, when the sputtering rate was included in the evaluation. More recently also sintered material for nitrogen calibration (AlN mixed with Al and Si3N4 mixed with Cu) was produced and points to a matrix independent emission yield of nitrogen T2 - 04 IGDSS CY - Berlin, Germany DA - 15.04.2018 KW - Glow Discharge KW - Non metals PY - 2018 AN - OPUS4-46223 LA - eng 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 - CONF A1 - Traub, Heike A1 - Saatz, Jessica A1 - Ascher, Lena T1 - Elemental imaging by laser ablation ICP-MS N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is nowadays an established multi-elemental analysis and mapping technique. It was shown that LA-ICP-MS can visualize the elemental distribution within tissue thin sections or cell samples. Quantification is possible by using appropriate matrix-matched calibration samples. Besides naturally occurring elements and metals from contrast agents, biomolecules using metal-tagged antibodies were detected in different bio-medical samples. By combining the results with findings from histology, magnetic resonance imaging (MRI) and other techniques disease related changes like alterations of the extracellular matrix can be investigated. T2 - 4th Colloquium of CRC 1340 "Matrix in Vision" CY - Berlin, Germany DA - 09.04.2019 KW - Laser ablation KW - ICP-MS KW - Imaging PY - 2019 AN - OPUS4-47752 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roethke, A. A1 - Görlitz, V. A1 - Jährling, R. A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Richter, Silke A1 - Rienitz, O. A1 - Schiel, D. T1 - SI-traceable monoelemental solutions on the highest level of accuracy: From the foundation of CCQM to recent advances N2 - Shortly after founding the CCQM in 1993, the first key comparison (CCQM-K2) about the determination of Cd and Pb content in river water was hosted by IRMM. It has been clear from the beginning that for the determination of an element mass fraction in a matrix, accurate reference solutions would be the key point for a metrologically sound analysis. Triggered by the not entirely satisfactory results it was decided to investigate the basis of all measurements: the reference solutions. Thus in 1999, CCQM-K8, hosted by EMPA/LNE, started the tedious but indispensable work on elemental solutions standards. Additionally, PTB, BAM and Merck KGaA initiated a project to establish a traceability system for inorganic analysis based on accurate monoelemental solutions. Within this unique approach ten high purity reference materials were fully characterized, and solutions were prepared gravimetrically thereof. These materials (forming the primary standards of elemental analysis) are available for NMIs/DIs from BAM. CCQM-P46 (Cu, Mg, Rh) demonstrated the actuality of the topic and the challenges to prepare elemental solutions for every element. The accurate preparation and use of monoelemental solutions is consequently reflected in the recurrent conduct of (key) comparisons: CCQM-P149 (purity of zinc), CCQM-K87 (Co, Cr, Pb), and the current CCQM-K143/P181 (Cu solutions), to name only a few in a long series. Is it necessary to put so much effort into the preparation of reference solutions? It clearly is! An example outside the world of academia: Recently, EDQM*, PTB, BAM and JRC have developed monoelemental reference standards traceable to the SI for toxic elements in support of the chapters of the European Pharmacopoeia, related to the analysis of elemental impurities in medicinal products. A new ICP OES method has been established allowing the comparison of two 1 g/kg mercury solutions with an outstandingly small uncertainty of Urel(w(Hg)) = 0.16 %. However, this technical progress would not have been possible without the ongoing effort of the metrological community within 25 years of research in the field of high accuracy monoelemental solutions. * EDQM: European Directorate for the Quality of Medicines and HealthCare T2 - CCQM Workshop on Advances in Metrology in Chemistry and Biology CY - Sevre DA - 10.04.2019 KW - CCQM KW - SI-traceable KW - Monoelemental solutions PY - 2019 UR - https://youtu.be/iVLk8CFnJTI AN - OPUS4-47846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis N2 - Wie kann Nicht-Messbares messbar gemacht werden? Die Antwort der Dissertation auf diese zentrale Frage der analytischen Chemie lautet: die Anwendung der hochauflösenden optischen Spektroskopie der diatomischen Moleküle. In der Arbeit wird in einem ersten Schritt in Grafitöfen, die wie Chemiereaktoren funktionieren, und durch die Anwendung verschiedener analytischer Methoden die diatomische Molekülbildung nachvollzogen. In einem zweiten Schritt werden die aufgedeckten Mechanismen auf die Bestimmung von Nichtmetallen und die Analyse von Isotopen angewendet. Die Isotopenanalytik ist das zukunftsweisendes Herzstück der Dissertation und von alltäglicher und politischer Relevanz: Mittels dieser Technik lässt sich die Herkunft von Lebensmitteln aber auch Chemiewaffen kostengünstiger und wesentlich schneller bestimmen als mit bisherigen Methoden der Massenspektrometrie. Möglich ist die Bestimmung, da alles um uns herum aus Atomen verschiedener Elemente besteht und die meisten Elemente mehrere Isotope haben. Isotope unterscheiden sich hinsichtlich ihres Gewichts, da sie über eine unterschiedliche Anzahl an Neutronen verfügen. Die Informationen über das Verhältnis von schweren und leichten Isotopen lässt sich nutzen, um zu bestimmen wo etwas entstanden ist. Jeder Ort auf unserem Planeten hat seinen persönlichen Element- und Isotopenanteil (Isotopenfingerabdruck). Das in der Arbeit angewandte Instrument misst das Verhältnis indirekt und nutzt hierzu die Interaktion zwischen Licht und Materie. Für das schwerere Isotop wird mehr Licht/Energie benötigt, um es in Bewegung zu bringen, als für das leichtere. Diese kleinen Unterschiede an Energie, die wir dafür aufwenden müssen, werden gemessen und ermöglichen die Herkunftsbestimmung. Damit leistet die Arbeit nicht nur einen wichtigen Beitrag zur Grundlagenforschung in der analytischen Chemie, sondern kann mit den aufgezeigten Ergebnissen auch Anwendung in den Bereichen Verbraucherschutz, Umweltforschung und Waffenkontrolle finden. N2 - The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis. First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios. T2 - Applied Photonics Award 2020 CY - Jena, Germany DA - 22.09.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie PY - 2020 AN - OPUS4-51996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Non-metals in inorganic reference materials N2 - The analysis of non-metals normally is carried out using elemental analysers which require reference material for calibration. In the lecture the CRM-program of BAM suitable for non-metal-analysis is presented. There are CRMs available with non-metal contents in the low ppm up to the high percent region. T2 - CETAMA 2018 CY - Paris, France DA - 27.11.2018 KW - CRM KW - Non-metals KW - Carbon KW - Sulfur KW - Oxygen KW - Nitrogen KW - Hydrogen KW - Reference material PY - 2018 AN - OPUS4-46968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - On developments of continuum source atomic and molecular absorption spectrometry N2 - Der Bunsen-Kirchhoff-Preis 2022 wurde am 23.06.2022 anlässlich der analytica conference in München an Dr. Carlos Abad verliehen - in Anerkennung seiner exzellenten Entwicklungen im Bereich der continuum source atomic absorption spectrometry (CS-AAS). Dr. Carlos Abad ist ein herausragender Experte auf dem Gebiet der Atom- und molekularen Absorptionsspektrometrie. insbesondere trug er maßgeblich zur substanziellen Weiterentwicklung von Echelle-Spektrometern für die CS-AAS bei. So gelang es, einen quantitativen Zugang zu Elementen wie Bor, Chlor, Fluor und Schwefel, mittels AAS zu erreichen. Erstmals demonstriert Dr. Carlos Abad am Beispiel eines Zr-Modifier, dass durch die Zeitauflösung der eingesetzten Echelle-Systeme mechanistische Untersuchungen zur Wirkung des Modifiers im Graphitrohrofen möglich sind. Besonders hervorzuheben sind seine Arbeiten zum Einsatz der CS-AAS für die Analyse von Isotopen, die eine Genauigkeit aufweist, welche an die der Multikollektor-induktiv gekoppelten Plasma-Massenspektrometrie (MC-ICP-MS) heranreicht. Damit ergeben sich völlig neue Einsatzmöglichkeiten für technologisch hochrelevante Applikationen, wie z.B. die Untersuchung der Alterung von Lithium-Batterien oder die Lithium-Analyse in Blutserum. T2 - Analytica Conference: Bunsen-Kirchhoff-Preis 2022 der Deutsche Arbeitskreis für Analytische Spektroskopie (DAAS) CY - Munich, Germany DA - 23.06.2022 KW - Isotopes KW - Fluorine KW - Halogens KW - Non-metals KW - HR-CS-MAS KW - HR-CS-AAS KW - Bunsen-Kirchhoff-Preis KW - Continuum source atomic absorption spectrometry KW - Zr-Modifier KW - Graphite furnace KW - Lithium PY - 2022 AN - OPUS4-56500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Origin, Provenance, and Isotope analysis N2 - Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice. All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis. T2 - Berlin Sciendce Week – Zukunftsorte – Innovation Made in Berlin CY - Berlin, Germany DA - 07.11.2019 KW - Isotope analysis KW - Optical spectroscopy KW - Provenance KW - Iisotopic signature KW - Isotopic fingerprints PY - 2019 AN - OPUS4-49889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Advantages of N2-MICAP-MS for Trace Metal Analysis in Steel N2 - The climate and energy crisis are extreme challenges. One possible solution could be hydrogen technology. Safety is a big concern. Steel used for pipelines and storage is under permanent stress from low temperatures and high pressures. The content of different alloyed metals determines the performance of the steel. Nitrogen microwave inductively coupled atmosphere pressure plasma mass spectrometry (N2-MICAP-MS) is a promising method for trace metal analysis in steel. Nitrogen is cheap and can be generated on site. It has fewer interferences than argon. Additionally, MICAP-MS is very matrix tolerant, proving the matrix-matched calibration expendable. Safety in technology and chemistry is the mission of BAM. Providing reference methods and materials can create trust in future technologies like hydrogen. T2 - SALSA Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - Trace analysis KW - Steel KW - Microwave plasma KW - Mass spectrometry KW - Safety PY - 2022 AN - OPUS4-55792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope ratio working group at CCQM N2 - The presentation gives the reasons for initiation of an isotope ratio working group at CCQM level, describes the process and provides the auduince with the initial working plan. T2 - EURAMET TC-MC Workshop on Isotope Ratio Analysis CY - Bern, Switzerland DA - 05.02.2020 KW - Metrology KW - Absolute isotope ratio KW - Isotope ratio KW - Delta value PY - 2020 AN - OPUS4-50344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Pb isotope ratio analysis N2 - The determination of Pb isotope ratios by TIMS and ICP-MS is discussed and applications from archaeology are provided. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope reference material KW - Provenance KW - Silver artefacts KW - Curse tablets PY - 2023 AN - OPUS4-59167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Measurement Uncertainty in Isotope Ratio Measurements N2 - The importance for measurement uncertainty in isotope ratio measurements is expalined and different approaches for calculating measurement uncertainty for absolute isotope ratios, isotope deltas and conventional isotope ratios are presented. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope delta KW - Absolute isotope ratio KW - Conventional isotope ratio PY - 2023 AN - OPUS4-59169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Sr isotope ratio analysis N2 - The measurment of Sr isotope ratios is described and examples from food authenticity, provenancing of cement and pietas are provided. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Conventional isotope ratios KW - Gypsum KW - Cement KW - Cheese PY - 2023 AN - OPUS4-59168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Detector deadtime N2 - Deadtime effects for counting detectors in ICP-MS and deadtime correction are discussed. Approaches for determining the deadtime are presented. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Counting detector KW - Detector deadtime KW - Isotope ratio KW - Dual mode detector PY - 2023 AN - OPUS4-59166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope Ratio Analysis N2 - Basic information on isotope ratio analysis is provided. Isotope fractionation is discussed and the measurement process is described. Additionally, practical examples are provided. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope fractionation KW - Mass spectrometry KW - Terminology PY - 2023 AN - OPUS4-59164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander A1 - Wichser, A. A1 - Abad Andrade, Carlos Enrique A1 - Bleiner, D. T1 - How does solid microanalysis profit from innovations in EUV research N2 - Research into new sources for EUV lithography is driving advancements in experimental methods tailored for this short wavelength range. This progress enables the exploration of spectroscopic techniques aimed at monitoring electronic transitions within this energy spectrum. Laser-induced breakdown spectroscopy (LIBS) serves as a rapid tool for elemental analysis, primarily established in the UV-vis range. However, LIBS encounters challenges such as limited repeatability precision and elevated background noise resulting from continuum radiation. In parallel, laser-induced extreme UV spectroscopy (LIXS) delves into the initial stages of plasma evolution, characterized by the emergence of soft X-ray and extreme UV radiation. The method benefits from a fast timeframe and constrained plasma confinement, leading to better precision. Nevertheless, LIXS encounters convoluted spectra arising from unresolved transition arrays (UTA), particularly pronounced for heavier elements. This complexity renders conventional univariate data analysis impractical, demanding the adoption of a multivariate data analysis approach. Multiple cathode samples, each coated with varying stoichiometries of lithium nickel manganese cobalt oxide (NMC), were prepared and used for calibration purposes. Through the application of Partial Least Squares (PLS) regression, a robust correlation with an R2 value exceeding 0.97 was achieved. The LIXS technique underwent a comparative evaluation against UV-vis LIBS. Furthermore, a comparison between univariate and multivariate analysis approaches was conducted, incorporating validation through y-randomization to mitigate overfitting risks. The viability of this approach was confirmed through the testing of an NMC reference material. The results showed metrological compatibility with reference values, underscoring the potential capability of the proposed methodology. T2 - 322. PTB Seminar 2023 - VUV and EUV Metrology CY - Berlin, Germany DA - 14.11.2023 KW - Laser induced XUV spectroscopy KW - Lithium-ion batteries KW - Solid microanalysis PY - 2023 UR - https://www.euv2023.ptb.de/ AN - OPUS4-58834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope Ratio Measurement - Quantities and calibration N2 - The quantities and the terminoly in isotope ratio measurements is presented, followed by explaining calibration approaches for isotope ratio measurements. Sources of error and bias are presented and special focus is given on single detector mass spectrometry. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope fractionation KW - Matrix separation KW - Interferences KW - Noise KW - Optimization PY - 2023 AN - OPUS4-59165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander A1 - Wichser, A. A1 - Abad Andrade, Carlos Enrique A1 - Bleiner, D. T1 - Study of lithium-ion battery aging using laser-induced XUV spectroscopy (LIXS) N2 - Laser-induced XUV spectroscopy (LIXS) is an emerging technique for elemental mapping. In comparison to conventional laser-induced breakdown spectroscopy in UV-vis (LIBS), it has a higher precision and wider dynamic range, and it is well suited for the quantification light elements like lithium and fluorine. Further it can spot oxidation states. The XUV spectra are produced at a very early stage of the plasma formation. Therefore, effects from plasma evolution on the reproducibility can be neglected. It has been shown, that high-precision elemental quantification in precursor materials for lithium-ion batteries (LIBs) can be performed using LIXS. Based on these results, LIXS mapping was used to investigate aging processes in LIBs. Different cathode materials with varying compositions of fluorine containing polymer binders were compared at different stages of aging. Due to effects comparable to X-ray photoelectron spectroscopy but in reverse, monitoring of changes in the oxidation state is envisioned, which makes information about the chemical environment of the observed elements accessible. The combination of elemental distribution and structural information leads to a better understanding of aging processes in LIBs, and the development of more sustainable and safe batteries. T2 - Conference on Applied Surface and Solid Material Analysis - AOFKA 2023 CY - Zurich, Switzerland DA - 11.09.2023 KW - Lithium Ion Batteries KW - Laser-induced XUV spectroscopy KW - Multivariate data analysis PY - 2023 AN - OPUS4-58587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander A1 - Wichser, A. A1 - Abad Andrade, Carlos Enrique A1 - Bleiner, D. T1 - Multivariate data analysis for laser-induced XUV spectroscopy (LIXS) N2 - The application of multivariate data analysis is essential in extracting the full potential of laser-induced XUV spectroscopy (LIXS) for high-precision elemental mapping. LIXS offers significant advantages over traditional laser-induced breakdown spectroscopy in UV-vis (LIBS), including higher precision and a wider dynamic range,[1,2] while making it possible to determine light elements like lithium and fluorine. However, it is challenged by the presence of unresolved transition arrays (UTAs) for heavier elements. These UTAs add considerable complexity to the spectral data, often concealing crucial information. In this study, we employ well-established multivariate data analysis techniques and intensive data preprocessing to unravel this contained information. The refined analysis reveals a high level of detail, enabling the precise identification of inhomogeneities within material samples. Our approach has particular relevance for studying aging processes in lithium-ion batteries (LIBs), specifically in relation to varying cathode materials and fluorine-containing polymer binder content. By combining elemental distribution with structural information, this improved method can offer a more comprehensive understanding of sample inhomogeneities and aging processes in LIBs, contributing to the development of more reliable and sustainable battery technologies. T2 - Berliner Chemie in Praxis Symposium - BCPS 2023 CY - Berlin, Germany DA - 06.10.2023 KW - Lithium Ion Batteries KW - Laser-induced XUV spectroscopy KW - Multivariate data analysis PY - 2023 AN - OPUS4-58588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotope analysis by high-resolution optical spectroscopy: a tool for planetary science N2 - Isotope analysis can be used to determine the age and provenance of geological samples. Modern techniques in optical spectrometry allow us a stand-off isotope analysis. This seminar will discuss how planetary science with the next Moon and Mars missions drive optical spectrometry into precise and accurate isotope analysis and how BAM will contribute. T2 - Adlershofer Kolloquium CY - Online meeting DA - 19.05.2020 KW - Provenance KW - Dating KW - Isotopes KW - Optical spectroscopy KW - Isotopic shift KW - Planetary science PY - 2020 AN - OPUS4-51995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander A1 - Abad Andrade, Carlos Enrique A1 - Morcillo, Dalia A1 - Riedel, Jens A1 - Okumura, M. T1 - Anwendung von hochauflösender optischer Spektrometrie zur Lithium-Isotopenanalyse N2 - Optische Spektrometrie wird als Alternative zur Massenspektrometrie im Bereich der Lithium-Isotopenanalyse vorgestellt. T2 - 11. Analytische Tage CY - Idstein, Germany DA - 11.05.2023 KW - Lithium KW - Isotopenanalyse KW - Atomabsorptionsspektrometrie KW - Massenspektrometrie PY - 2023 AN - OPUS4-57543 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Breaking the wall of uncertain origin N2 - Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice. All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis. T2 - Falling Walls Lab Adlershof CY - Berlin, Germany DA - 27.09.2019 KW - Isotope analysis KW - Optical spectroscopy KW - Provenance PY - 2019 AN - OPUS4-49882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pramann, A. A1 - Vogl, Jochen A1 - Flierl, L. A1 - Rienitz, O. T1 - Determination of absolute (SI‐traceable) isotope ratios: The use of Gravimetric Isotope Mixtures N2 - The presentation is brief overview on how to use gravimetric isotope mixtures to determine SI traceable isotope ratios. There is no mass spectrometer on earth that directly measures isotope ratios. Mass spectrometers will always measure signal intensity ratios instead. The actual problem is that the measured intensity ratios differ more or less from the isotope ratios. The difference can be up to more than 10 % in case of lithium while it‘s below 1 % in case of the heavier elements like lead or uranium. Consequently, the signal intensity ratios are expressed for example in V/V depending on the type of mass spectrometer you are using, while the isotope ratios are expressed in mol/mol. This phenomenon is called Instrumental Isotopic Fractionation (or short IIF) but the more common name is still mass bias (even though this name is not entirely correct). To convert the measured into the isotope ratio usually a simple multiplication with a so-called correction (or short K) factor is done. Therefore, the problem is to determine the K factor. In absence of isotope reference materials the golden route is via gravimetric isotope mixtures, which will be explained within the presentation. T2 - CCRI-CCQM Workshop on the use of mass spectrometry in radionuclide metrology: Opportunities and challenges - Video Tutorial CY - Online meeting DA - 14.02.2023 KW - Absolute isotope ratio KW - Traceability KW - Uncertainty KW - Isotope mixtures PY - 2023 AN - OPUS4-57172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemke, Nora A1 - El-Khatib, Ahmed A1 - Theuring, F. A1 - Jakubowski, Norbert A1 - Vogl, Jochen T1 - Sulfur isotope dilution ICP MS for traceable protein quantification N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful method for the matrix-independent quantitative analysis of target elements. Developed for the use in inorganic trace analysis, ICP-MS is nowadays a valuable tool for bioanalytical questions. Especially the use of ICP-MS for quantitative proteomics by measuring heteroatoms has gained recognition in the last decade, considering that established quantification methods like organic mass spectrometry depend on labelling of the target protein or the existence of matched protein and peptide standards. The need for reliable quantification of proteins is continuously growing, but only a limited number of well-characterized and quantified protein standards are available so far. Accurately quantified, traceable protein standards are necessary to ensure comparability of measurements between laboratories, not only in basic research but also in a clinical context. One example of this is the Alzheimer’s disease biomarker tau protein. However, existing tau standards lack comparability, emphasizing the need for a well-quantified protein standard. Therefore, we developed a method for the quantification of pure proteins via sulfur isotope dilution ICP-MS (IDMS). As sulfur is present in two amino acids, cysteine and methionine, it exists in nearly all proteins and can be used for the quantification of proteins of known stoichiometry. We employed simple offline strategies for the separation of non-protein bound sulfur species. Quantification of these contaminations by IDMS allows for correction of the protein content and enables reliable protein quantification. We report the protein mass fractions of a standard reference material and commercially available proteins determined by sulfur IDMS, including the expanded uncertainties. The developed method can be applied for the reliable and traceable quantification of pure proteins for use as in-house standards. Here, we successfully used this method for the quantification of the tau protein. T2 - 53rd annual conference of the DGMS including 27th ICP-MS User's Meeting CY - Münster, Germany DA - 01.03.2020 KW - ICP-MS KW - Isotope dilution KW - Protein KW - Quantification KW - Tau protein PY - 2020 AN - OPUS4-50510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - The triple isotope calibration approach BT - A new calibration approach for obtaining absolute isotope ratios of multi-isotopic elements N2 - The calibration of isotope ratio measurements is an ongoing challenge since instrumental isotope fractionation (IIF) has been detected in mass spectrometry (MS). There is a variety of approaches which either bypass IIF such as delta measurements or refer to reference materials (RMs) and thus shifting the problem of calibration to somebody else: the RM producer. For certifying isotope RMs with absolute isotope ratios only a few approaches are available, namely the isotope mixture approach, the double spike approach, the mass bias regression model and total evaporation in TIMS. All of them require either enriched isotopes, isotope RMs of another element or an RM for correcting residual error. As the enriched isotopes required for the isotope mixture and the double spike approach need to be fully characterized beforehand, all mentioned calibration approaches require a standard. Here, a new and standard-free calibration approach for obtaining absolute isotope ratios of multi-isotopic elements has been developed. The underlying principle is that each MS suffers from IIF and thus yields a specific isotope fractionation line in a three-isotope diagram. When applying a second MS featuring a different ionization mechanism, we obtain a second isotope fractionation line with a different slope in the same three-isotope diagram. In both cases the absolute isotope ratios range somewhere on the isotope fractionation line. Consequentially, the intersect of both lines yield the absolute isotope ratios of the measured sample. This theory has been tested by measuring Cd and Pb isotope ratios of suitable isotope RMs with a TIMS and an ICP-MS, both equipped with multi-collector array. During the measurements the ionization conditions were changed such that different extent of the isotope fractionation has been achieved. With the resulting data set the theory described above could be verified. The obtained absolute isotope ratios were metrologically compatible with the certified isotope ratios. The remaining average bias of -5 ‰ can be reduced with further improvements. The calibration approach is universal and can be applied to any multi-isotopic element and it is not limited by the type of the mass spectrometer. T2 - Virtual Goldschmidt 2021 CY - Online meeting DA - 04.07.2021 KW - Absolute isotope ratio KW - Traceability KW - Metrology KW - Calibration KW - Uncertainty KW - Triple isotope fractionation PY - 2021 AN - OPUS4-53023 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-Begutachterschulung Modul E zur Akkreditierung von Eignungsprüfungsanbietern und Referenzmaterialherstellern CY - Online meeting DA - 04.02.2021 KW - ISO-Guide 35 KW - Referenzmaterial-Herstellung KW - ZRM PY - 2021 AN - OPUS4-52099 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - IRWG strategy update N2 - An update of the IRWG strategy for the period 2023-2030 is given. The status and the futuere work of the task group on quantities, symbols and units is discussed. The present status of IRWG comparisons is shown and the need for specific key comparisons is discussed. T2 - CCQM IRWG Meeting CY - Sevres, France DA - 24.04.2023 KW - Isotope ratio KW - Traceability KW - Metrology PY - 2023 AN - OPUS4-57400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemke, Nora A1 - El-Khatib, Ahmed A1 - Theuring, F. A1 - Vogl, Jochen A1 - Jakubowksi, Norbert T1 - Protein quantification of an Alzheimer’s biomarker via isotope dilution inductively coupled plasma mass spectrometry N2 - Neurodegenerative diseases are one of the major problems for our ageing society. Alzheimer’s disease (AD) as the most common neurodegenerative disorder affects over 46.8 million people worldwide and the number will increase as the population ages. The diagnosis of AD is challenging and only half of the patients are identified yet and often only in late stages. One reason is that existing assays for identification and quantification of AD biomarkers lack accuracy and are poorly comparable. This study is part of the EU project “ReMiND” aiming to develop accurate, reliable and traceable methods for the detection and quantification of known and suspected AD biomarkers. Our target is the tau protein, as brain load and distribution of tau is highly correlated with the clinical progression of AD. We intend to develop a measurement method for the accurate quantification of tau by means of inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS is a powerful method for the matrix independent quantitative analysis of target elements. Developed for the use in inorganic trace analysis, ICP-MS is nowadays emerging as a valuable tool for bioanalytical questions. Especially the use of ICP-MS for quantitative proteomics by measuring heteroatoms is highly promising, considering that established quantification methods like organic mass spectrometry depend on the existence of matched protein and peptide standards or labelling of the target protein. In this work, we applied isotope dilution analysis (IDA) using ICP-MS to quantify proteins of known stoichiometry via their sulphur content. Sulphur is present in two amino acids, cysteine and methionine, and hence is omnipresent in nearly all proteins. A NIST standard bovine serum albumin (BSA) was quantified using sulfur IDA to optimize sample preparation and method parameters. Our goal is to employ the developed method in a proof of concept study for the quantification of the AD biomarker tau extracted from brains of a mouse model for AD. T2 - 26. ICPMS-Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - ICP-MS KW - Isotope dilution KW - Protein analysis PY - 2018 AN - OPUS4-46585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - How Online NMR Spectroscopy Accelerates Chemical Process Development and Manufacturing – From Automated Spectral Analysis to Integrated NMR Micro Reactors N2 - Accelerating chemical process development and manufacturing along with quick adaption to changing customer needs means consequent transformation of former batch to continuous (modular) manufacturing processes. These are justified by an improved process control through smaller volumes, better heat transfer, and faster dynamics of the examined reaction systems. As an example, for such modular process units we present the design and validation of an integrated nuclear magnetic resonance (NMR) micro mixer tailor‐made for a desired chemical reaction based on computational modelling. The micro mixer represents an integrated modular production unit as an example for the most important class of continuous reactors. The quantitative online NMR sensor represents a smart process analytical field device providing rapid and non‐invasive chemical composition information without need for calibration. We describe the custom design through computational fluid dynamics (CFD) for the demands of the NMR sensor as well as for the given reaction conditions. The system was validated with an esterification reaction as an example for a chemical reaction process. Systems utilizing such an online NMR analyser benefits through short development and set‐up times based on “modular” spectral models. Such models can simply be built upon pure component NMR spectra within minutes to a few hours (i.e., assignment of the NMR signals to the components) instead of tedious DoE calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). The approach was validated for typical industrial reactions, such as hydrogenations or lithiations. T2 - Wissenschaftliches Kolloquium des Leibniz-Institut für Katalyse e. V. an der Universität Rostock CY - Rostock, Germany DA - 09.10.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Data Analysis KW - Digitization KW - Catalysis PY - 2019 AN - OPUS4-49238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -