TY - CONF A1 - Riedel, Soraya A1 - Talke, A. A1 - Lisdat, F. T1 - Enzyme activity determination of human monoamine oxidase B (Mao B) by amperometric hydrogen peroxide detection N2 - Parkinson’s disease (PD) is one of the most common neurodegenerative disorders worldwide. About 0.3 % of the global population and approximately 2 % of people older than 80 years are affected by PD. Monoamine oxidase B (Mao B) is an enzyme, which is a drug target in Parkinson’s disease (PD), since it is involved in dopamine metabolism. Several Mao B inhibitors are well established as medication for PD patients. However, the medical treatment is only little personalized since the monitoring of the patients Mao B activity is complex and requires sophisticated laboratory equipment. Here a sensorial Mao B activity determination system has been developed which has potential in the personalization of the medical PD treatment. The enzyme activity is quantified by amperometric detection of enzymatically produced H2O2. Therefore, the enzyme is enriched from the solution via cellulose particles which are functionalized with antibodies against human Mao B. The successful capturing of the enzyme can be verified by SDS-PAGE. For activity determination the enzyme is brought in contact with a suitable substrate - here benzylamine. Selectivity of the amperometric hydrogen peroxide detection in the presence of co-reactants has been verified. Within the time span of 30 min, a linear dependency of enzymatically produced H2O2 with the substrate incubation time can be observed. This allows the evaluation of the Mao B activity. The results have been correlated to an optical detection method. Furthermore, the method has been tested for different amounts of enzyme used in the experiments and found to be sensitive enough for Mao B analysis in blood samples. T2 - European Biosensor Symposium 2021 CY - Online meeting DA - 09.03.2021 KW - Monoamine oxidase B KW - Amperometry KW - Prussian blue KW - Parkinsons's disease KW - Screen-printed electrodes PY - 2021 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-52270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Von Elementspezies, Isotope und Zellen oder: wie kommt man eigentlich von Westfalen nach Berlin N2 - Im Rahmen des Vortrages werden die Möglichkeiten der Elementanalytik an Applikationsbeispielen aus Umwelt und life-sciences aufgezeigt. Hierbei kommen ICP-MS Kopplungstechniken, stabile Isotope und Einzellen- und Partikelanalytik (sc-/sp-ICP-ToF-MS) zum Einsatz. T2 - DAAS PhD Seminar CY - Online meeting DA - 20.09.2021 KW - Elementspezies & Isotope KW - ICP-MS & HR-CS-GFMAS KW - Kopplungstechniken PY - 2021 AN - OPUS4-53378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Faßbender, Sebastian A1 - Rodiouchkina, K. A1 - Vanhaecke, F. 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 using a multiple-injection approach for instrumental mass bias correction by standard-sample bracketing. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared to data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was promising regarding the differentiation of the river systems by the isotopic signature of river water sulfate. The great potential of this method is based on the versatility of the applied separation technique, not only in the environmental field but also for, e.g., biomolecules, as sulfur is the only covalently bound constituent of proteins that can be analyzed by MC-ICP-MS. T2 - 12th International Conference on Instrumental Methods of Analysis-Modern Trends and Applications (IMA) CY - Online meeting DA - 20.09.2021 KW - CE/MC-ICP-MS KW - Species-specific Isotope Analysis KW - Environmental & life science application KW - Speciation Analysis PY - 2021 AN - OPUS4-53379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Langenhan, Jennifer A1 - Lisec, Jan A1 - Jaeger, Carsten T1 - PEGomics: A meta-study on factors affecting polyethylene glycol (PEG) levels in human blood N2 - Polyethylene glycols (PEGs) are widely used in everyday items such as food additives and in personal care products. In addition, they have multiple medical applications: as laxatives, excipients, and covalently coupled to drug molecules leading to improved pharmacokinetics (PEGylation). While generally regarded as biologically inert, the human body is known to produce antibodies against PEGylated molecules. In addition, PEGs have been shown to be part of a biomarker signature to predict colon cancer outcome, suggesting a more complex and yet unknown behavior of PEGs in the human body. Here, we introduce PEGomics, a retrospective screening approach of publicly available LC-MS data. Using a custom R script to process entire studies, the presence of PEGs was reveled in most human plasma, serum and whole blood samples investigated. Several PEG species and adducts were identified and their correlation with different diseases and health conditions was investigated further. Blood PEG levels significantly differed between patient groups in multiple clinical studies related to e.g. pregnancy duration, fasting and smoking. We discuss possible causes for these effects in the light of recent reports of allergies against PEGs and outline our further strategies to identify the source of PEGs in the human body as well as possible metabolic transformations. T2 - ACS Spring 2021 CY - Online meeting DA - 05.04.2021 KW - PEG KW - Polyethylene glycole KW - PEGomics KW - Retrospective analysis KW - Meta-study PY - 2021 AN - OPUS4-53392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - HR-CS-GFMAS for PFAS sum parameter analysis in surface water and soil samples N2 - Vorstellung neuer HR-CS-GFMAS basierter Analysemethoden zur Analytik von PFAS in Oberflächenwasser und Boden. T2 - 2. Online-Workshop "Emissionsmessverfahren für per- und polyfluorierte Chemikalien (PFC)" CY - Online meeting DA - 30.09.2021 KW - HR-CS-GFMAS KW - PFAS KW - Oberflächenwasser und Boden PY - 2021 AN - OPUS4-53465 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Veiko, V. P. A1 - Karlagina, J. J. A1 - Polyakov, D. S. A1 - Samokhvalov, A. A. T1 - Reverse deposition of TI-oxides under nanosecond laser ablation of TI N2 - Processes of laser induced oxidation of metals are typically studied in the framework of heterogeneous chemical reactions occurring on the irradiated surface, which lead to the formation of dense oxide films deposited on it. Such technology has many applications like color-laser marking technology and laser recording on thin metal films for creation of diffractive optical elements . Under the conditions of strong laser ablation, another oxidation mechanism becomes possible: evaporated atoms react with oxygen in a surrounding atmosphere and the products of such reaction are redeposited back onto the substrate. The chemical and phase composition of such deposited layer, its density, morphology and structure depend on the conditions of laser ablation. By varying these conditions, the main properties of such coating can be controlled that is important for some potential application (for example in biomedicine). In our report we present the study of the processes of redeposition of oxides structure under the conditions of multipulse nanosecond laser ablation of titanium (Grade 2) in air atmosphere at normal conditions. Our experiments show that titanium-implants with such deposited oxide layer have increased biocompatibility. Modelling of chemical reaction in laser-induced plasma coupled with experimental methods of plasma optical emission spectroscopy allows us to determine the types of main chemical reactions in laser plasma as well as it influences on the plume dynamics and vapor condensation kinetics. As a result, we propose the general physical picture of reverse deposition of oxides structure under the condition of strong nanosecond laser ablation. The formation of the titanium oxide precipitate is explained not only by collisions in the plasma, but also by the chemical interaction of titanium and oxygen, which leads to the formation of а low pressure area near the substrate and additionally stimulates the reverse deposition of oxides. We expect, similar processes are valid not only for titanium but also for other metals and, possibly, semiconductors. T2 - 28th International Conference on Advanced Laser Technologies CY - Online meeting DA - 06.09.2021 KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Emission spectroscopy KW - Titanium dioxide KW - Hydrodynamic model KW - Plasma chemistry PY - 2021 AN - OPUS4-53245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - von der Au, Marcus A1 - Meermann, Björn T1 - Untersuchung von PFAS-Summenparameter-Methoden Vergleich zwischen AOF vs. EOF und CIC vs. HR-CS-GFMAS N2 - Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse mit über 5200 Verbindungen. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“. Die PFAS-Analytik ist wegen den vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. Weiterhin wird die Analytik aufgrund der Substitution von bereits regulierten PFAS mit ständig steigenden Anzahlen an PFAS-Verbindungen in der Umwelt konfrontiert. PFAS-Summenparameter-Methoden, die ein nahezu vollständiges Abbild der PFAS-Belastungssituation wiedergeben, werden daher immer wichtiger. In unserer Studie haben wir die zwei meistverwendeten PFAS-Summenparameter, das adsorbierbare organisch gebundene Fluor (AOF) und das extrahierbare organisch gebundene Fluor (EOF), miteinander verglichen. Beide Summenparameter können zur Analyse mit entweder combustion-Ionenchromatographie (CIC) oder hochauflösender Molekülabsorptionsspektrometrie (HR-CS-GFMAS) gekoppelt werden. Hierbei diskutieren wir die Vor- und Nachteile sowohl von beiden Summenparameter- als auch beider Detektions-Methoden. Die Untersuchungen wurden mit Oberflächenwasserproben aus der Spree in Berlin durchgeführt. Neben AOF und EOF wurde auch der Gesamt-Fluorgehalt (TF) mit CIC sowie HR-CS-GFMAS bestimmt. Die Fluor-Massenbilanzierung zeigte, dass das Verhältnis AOF/TF höher als das Verhältnis EOF/TF war. Dabei machte der AOF 0.14–0.81% vom TF und der EOF 0.04–0.28% vom TF aus. Insgesamt war die neue EOF/HR-CS-GFMAS-Methode schneller, präziser und sensitiver als die bereits etablierte AOF/CIC-Methode. Beide Methoden sind vielversprechend für die zukünftige Überwachung von Umweltproben und bilden die Grundlage für mögliche Grenzwerte, die auf die Summe PFAS abzielen. T2 - Umwelt 2021 CY - Online meeting DA - 07.09.2021 KW - PFAS KW - HR-CS-GFMAS KW - CIC KW - AOF KW - EOF KW - Fluor PY - 2021 AN - OPUS4-53226 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Meermann, Björn T1 - Erfassung der PFAS-Belastungssituation in Umweltproben - Schnelle & sensitive PFAS-Summenparameteranalytik mittels HR-CS-GFMAS N2 - In der Verbindungsklasse der per- und polyfluorierte alkylischen Substanzen (PFAS) werden über 5200 organische Verbindungen zusammengefasst. PFAS sind an mindestens einem Kohlenstoffatom vollständig fluoriert. Sie werden mit negativen Einflüssen auf die menschliche und tierische Gesundheit assoziiert, sind extrem persistent in der Umwelt und bioakkumulieren entlang von Nahrungsnetzen. Daher zählen PFAS zu den „emerging pollutants“. Gleichzeitig machen ihre physikalisch-chemischen Eigenschaften sie für die Verwendung in diversen technischen Anwendungen attraktiv. Sie sind sowohl hydro- als auch lipophob und zeigen durch die starke C-F-Bindung hohe thermische wie chemische Beständigkeit. Erste Regulierungen einiger PFAS in Kombination mit den technisch hervorragenden Eigenschaften erzeugt einen Innovationsdruck und führten zu einem enormen Anstieg in der Zahl der Substitutionsverbindungen. Auf Grund der steigenden Komplexität der Substanzklasse ist die Target-Analytik nicht in der Lage eine solche Vielfalt und Vielzahl an Analyten zu erfassen. Für eine akkurate Erfassung der Belastungssituation durch PFAS, die Identifikation von PFAS-Hotspots und eine Bewertung von geeigneten Sanierungsmaßnahmen ist daher eine geeignete PFAS-Summenparameteranalytik notwendig. Daher geben wir hier Einblicke in den aktuellen Stand der PFAS-Summenparameterentwicklung und präsentieren unsere neusten Ergebnisse zur Methodenentwicklung für die quantitative Analyse von PFAS als extrahierbares organisch gebundenes Fluor (EOF) in Umweltproben mittels hochauflösender Molekülabsorptionsspektrometrie (HR-CS-GFMAS). Hierfür optimierten wir die Extraktion von PFAS aus verschieden Feststoff-Matrizes bei zeitgleicher Abtrennung anorganischen Fluorids. Durch den Zusatz von Galliumsalz-Lösungen als modifier in der HR-CS-GFMAS kann Fluor indirekt sehr selektiv durch die in situ Bildung von GaF sehr nachweisstark (instrumentelle LOQ ~3 µg/L) quantifiziert werden. T2 - Umwelt 2021 CY - Online meeting DA - 07.09.2021 KW - Per- and polyfluorinated alkyl substances (PFASs) KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Solid phase extraction (SPE) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction KW - Böden PY - 2021 AN - OPUS4-53227 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Meermann, Björn T1 - Finding the most suitable PFASs sum parameter method - A Comparison of AOF vs. EOF and CIC vs. HR-CS-GFMAS N2 - Since it is unknown for many applications, which PFASs are used and how they enter the environment, target analysis-based methods reach their limits. The two most frequently used sum parameters are the adsorbable organically bound fluorine (AOF) and the extractable organically bound fluorine (EOF). Both can be quantified using either combustion ion chromatography (CIC) or high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Here we provide an insight on the advantageous and disadvantageous of both sum parameters and both detection methods. Our study is based on the analysis of surface water samples. Next to total fluorine (TF) analysis, AOF and EOF were determined as well as CIC and HR-CS-GFMAS are compared and results are comparatively discussed. Fluorine mass balancing revealed that, the AOF/TF proportion was higher than the EOF/TF proportion. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF. Although, organically bound fluorine represents only a small portion of TF, PFASs are of worldwide concern, because of their extreme persistence and their bioaccumulation potential. The EOF-HR-CS-GFMAS method turned out to be more precise and sensitive than the AOF-CIC method and is a promising tool for future monitoring studies/routine analysis of PFASs in the environment. T2 - Emerging Contaminants in the Environment Conference CY - Online meeting DA - 27.04.2021 KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Combustion ion chromatography (CIC) KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Adsorbable organically bound fluorine (AOF) KW - Extractable organically bound fluorine (EOF) PY - 2021 AN - OPUS4-53228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, A. A1 - Lischeid, G. A1 - Koch, Matthias A1 - Lentzsch, P. A1 - Müller, M.E.H. T1 - Priority effects influence the production of mycotoxins of Fusarium and Alternaria N2 - Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads. Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria tenuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9). Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies. T2 - 42. Mycotoxin Workshop CY - Online meeting DA - 30.05.2021 KW - Microbe interactions KW - Antagonists KW - Mycotoxins PY - 2021 AN - OPUS4-52815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Von der Au, Marcus T1 - HR-CS-GFMAS as a promising new tool for the analysis of organo-fluorine in environmental samples N2 - New HR-CS-GFMAS based methods for organically bound fluorine detection in environmental samples. T2 - CRC Colloquium - CRC 1349 Fluorine-Specific Interactions CY - Online meeting DA - 21.06.2021 KW - HR-CS-GFMAS KW - Organically bound fluorine KW - Fluorine sum parameter KW - Environmental analysis PY - 2021 AN - OPUS4-52844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - von der Au, Marcus A1 - Meermann, Björn T1 - A fast and simple extraction method for the determination of PFASs in soil samples - HR-CS-GFMAS a new screening tool N2 - Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future. T2 - ENSOr - International Workshop on Emerging policy challenges on new soil contaminants CY - Online Meeting DA - 06.05.2021 KW - PFAS KW - HR-CS-GFMAS KW - Soil KW - Sediment PY - 2021 AN - OPUS4-52608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Elemental analytical methods in material- & environmental analysis N2 - Materials in contact with the environment release e.g., metal-ions, elemental species and/or (nano-)particles. Once these species and/or particles are released, they are ingested by organisms and cells and thus, might have a negative impact on the environment. Thus, identification as well as quantification of potentially harmful substances is of utmost importance and highly needed to assess ecotoxicological impact of (emerging) pollutants. The oral presentation provides an overview on the power of elemental analytical techniques, in particular: ICP-MS as well as HR-CS-GFMAS in environmental research. Current research topics will be highlighted: i) Elemental Speciation analysis of anti-fouling agents via CE/MC-ICP-MS; ii) Per- and polyfluorinated compounds in surface waters via high resolution-continuum source-graphite furnace molecular absorption spectroscopy (HR-CS-GFMAS); iii) Single cell and single organism analysis via sc-ICP-ToF-MS and ETV/ICP-MS for ecotoxicological assessment. T2 - Analytical Colloquium at MERCK CY - Online meeting DA - 19.04.2021 KW - HR-CS-GFMAS KW - ICP-ToF-MS KW - ETV/ICP-MS PY - 2021 AN - OPUS4-52566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dinter, Adelina-Elisa A1 - An-Stepec, Biwen A1 - Wurzler, Nina A1 - Koerdt, Andrea A1 - Meermann, Björn T1 - Development of a single cell-ICP-ToF-MS-method for multielement analysis of MIC organisms grown on solid steel samples N2 - The latest ICP-MS technology - ICP-ToF (time of flight)-MS – enables the analysis of the multi-element fingerprint of individual cells. The interface between material and environmental analysis thus receives special attention, e.g., when considering corrosion processes. Microbiologically influenced corrosion (MIC) is a highly unpredictable phenomenon due to the influence of the environment, microbial communities involved and the respective electron source. However, the interaction pathway between cells and the metal surface remains unclear. The development of the MIC-specific ICP-ToF-MS analytical method presented here at the single cell level, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis and will enable clarification of the processes taking place. For this, a MIC-specific staining procedure was developed. It allows the analysis of archaea at a single cell level and provides information about the interaction of the cells with the staining agent which is extremely scarce compared to other well characterized organisms. Additionally, the single cell ICP-ToF-MS is used for the analysis of archaea involved in MIC of steel. Hence, the possible uptake of individual elements from different steel samples is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials. T2 - DAAS Doktorandenseminar 2021 CY - Online meeting DA - 20.09.2021 KW - Sc-ICP-ToF-MS KW - Single cell analysis KW - Microbiologically influenced corrosion KW - Archaea PY - 2021 AN - OPUS4-53340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Meermann, Björn T1 - Detection of PFAS pollution in environmental samples - A Fast & sensitive PFAS sum parameter method using HR CS GFMAS N2 - The substance class of per- and polyfluorinated alkyl substances (PFAS) comprises more than 5300 organic compounds. PFAS are completely fluorinated on at least one carbon atom. They are associated with negative impacts on human and animal health, are extremely persistent in the environment, and bioaccumulate along food chains. Therefore, PFAS are classified as emerging pollutants. At the same time, their physicochemical properties make them attractive for use in diverse technical applications. They are both hydrophobic and lipophobic and show high thermal as well as chemical resistance due to the strong C-F bond. First regulations of some PFAS in combination with the technically excellent properties generated an innovation pressure and led to an enormous increase in the number of fluorinated substitution compounds. Due to the increasing complexity of this substance class, target analysis is not able to cover such a variety and multitude of analytes. Therefore, a suitable PFAS sum parameter method is necessary for an accurate detection of PFAS pollution in the environment, the identification of PFAS hotspots and an evaluation of appropriate remediation measures. Here we provide insights into the current state of PFAS sum parameter development and present our latest results on method development for the quantitative analysis of PFAS as extractable organically bound fluorine (EOF) in environmental samples using high-resolution molecular absorption spectrometry (HR-CS-GFMAS). For this purpose, we optimized the extraction of PFAS from different solid matrices with simultaneous separation of inorganic fluoride. For quantification resulting extracts were measured using a fluorine specific HR-CS-GFMAS method. By adding gallium salt solutions as modifiers in HR-CS-GFMAS, fluorine can be indirectly quantified very selectively by the in situ formation of GaF with low limits of quantification (instrumental LOQ c(F) < 3 µg/L). Here we will show results from real soil samples from sites with and without known contamination. T2 - 6. Doktorandenseminar des Deutschen Arbeitskreises für Analytische Spektroskopie (DAAS) CY - Online meeting DA - 20.09.2021 KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Soil KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction PY - 2021 AN - OPUS4-53333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - ESAS - CSSC CY - Brno, Czech Republic DA - 04.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - SALSA - Communicating Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbrich, Adelina-Elisa A1 - An-Stepec, Biwen A1 - Koerdt, Andrea A1 - Meermann, Björn T1 - Multielemental analysis of MIC organisms grown on solid steel samples by means of single cell-ICP-ToF-MS N2 - Inductively coupled plasma-time of flight-mass spectrometry (ICP-ToF-MS) enables the analysis of the multi-element fingerprint of individual cells due to a (quasi-)simultaneous detection of about 70 elements of the periodic table. The interface between material and environmental analysis thus receives special attention, e.g., when considering corrosion processes. Microbiologically influenced corrosion (MIC) is a highly unpredictable phenomenon due to the influence of the environment, microbial communities involved and the respective electron source. However, the interaction pathway between cells and the metal surface remains unclear. The development of the MIC-specific ICP-ToF-MS analytical method presented here, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis and will enable clarification of the processes taking place. For this, a MIC-specific staining procedure was developed which ensures the analysis of intact cells. It allows the studies of archaea at a single cell level which is extremely scarce compared to other well characterized organisms. Additionally, the single cell ICP-ToF-MS is used for the analysis of archaea involved in MIC of steel. Hence, the possible uptake of individual elements from different steel samples is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials research. T2 - DGMS Young Scientists Fall Meeting 2022 CY - Hünfeld, Germany DA - 28.09.2022 KW - Single cell KW - Microbiological influenced corrosion MIC KW - Sc-ICP-ToF-MS KW - Method development PY - 2022 AN - OPUS4-55910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - New possibilities in single cell analysis via ICP-ToF-MS – zooming into the region where materials meet environment N2 - Materials are key for our modern communities; current life seems nearly impossible without concrete, plastic and metal. In particular metals play important roles in all areas of our daily life - from building materials to high tech products. However, due to the increasing consumption of metals and corresponding waste production, an elevated release of metals from buildings and consumer goods into the environment takes place. Furthermore, metals in direct contact with the environment undergo corrosion processes which leads also to a release of metals into the (aquatic) environment. Besides this immediate metal release, the lifespan of products/buildings are substantially reduced – hence unnecessary economic costs arise. Thus, research in this regard is needed within the force field of metal/material  environment. However, to evaluate the environmental impact of materials as well as developing “safe” materials, new analytical methods are highly needed. One promising powerful tool in this regard is single cell-ICP-ToF-MS for multi-elemental analysis on a single cell/organism level. Within this presentation the concept, strength as well as challenge of single cell-ICP-MS are briefly introduced. Afterwards, two application examples are presented: (i) assessing the environmental impact of metals and (ii) the impact of the environment on metal-based materials and the derivation of potential environmental-friendly material protection strategies. These applications highlight the strength of new analytical approaches to explore the durability and safety of newly developed materials. Thus, analytical chemistry is one corner stone to transformation of modern society into circular economy (CEco). (i) Diatoms are located at the bottom of the food chain. Thus, toxicological relevant metals taken up by diatoms can possibly accumulate within the food web and cause harmful effects. Diatoms are a common test system in ecotoxicology. To investigate potential metal uptake and harmful effects on a single cell level, we developed an on-line single cell-ICP-ToF-MS approach for multi-elemental diatom analysis. Our approach is a new potential tool in ecotoxicological testing for metal-based materials. (ii) Next to classical corrosion processes, microorganisms are responsible for so called microbially influenced corrosion (MIC). MIC is a highly unpredictable process relying on the interaction pathways between cells and the metal surface. To shed light on MIC processes and derivate potential metal protection strategies, we applied single cell-ICP-ToF-MS for MIC research on a single bacteria/archaea level. It turned out that microorganism are taking up particular metals from alloys - thus, single bacteria-ICP-ToF-MS will enable the development of environmental friendly corrosion protection strategies. T2 - 10th Nordic Conference on Plasma Spectrochemistry CY - Loen, Norway DA - 12.06.2022 KW - sc-ICP-ToF-MS KW - Material - Environment interaction KW - Diatom, Bacteria PY - 2022 AN - OPUS4-55533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Faßbender, Sebastian A1 - Meermann, Björn T1 - Mercury speciation in sediments of industrially impacted water bodies in Northern Germany using SSID GC/ICP-ToF-MS N2 - Sediments and soils can act as sinks of species of inorganic mercury (Hg2+), while they are simultaneously sources of organic species, such as monomethylmercury (MMHg). Although the fraction of MMHg in total Hg of sediments is suggested to be only 0.1–1%, MMHg poses a threat for humans and wildlife due to its toxic properties, high bioaccumulation potential and the ability to pass the blood-brain barrier. One example of a highly Hg contaminated waterbody is the Finow Canal, the oldest artificial waterway still in operation in Germany. Here, Hg mass fractions of up to 100 µg/g were found in the sediment in previous studies. These are suggested to be associated with a chemical plant producing mercury-based seed dressings. Despite this high mass fraction of Hg, no Hg speciation studies have been conducted there up to now. In this study, Hg speciation in sediments of Finow Canal at locations before and after the known polluted site was conducted using species-specific isotope dilution (SSID) GC-ICP-ToF-MS. Mass fractions of up to 0.41 µg/g MMHg were determined. In addition, waterbodies around the initially polluted site were investigated and elevated concentrations were also determined around 14 km downstream. For MMHg analysis, the performance of ICP-ToF-MS for SSID GC/ICP-MS was compared with ICP-Q-MS and ICP-SF-MS. Here, isotope ratio precision was similar between the tested instruments. However, the (quasi-) simultaneous detection of the whole mass spectrum will probably offer a much higher precision of ICP-ToF-MS, when more than one isotope system is used. These results are the first evidence of the occurrence of MMHg in this region and show the need for further investigations of the whole regional ecosystem, as well as the consideration of possible measures of remediation. SSID GC-ICP-(ToF)-MS is a suitable tool for investigating species-specific (multi) isotope systems for environmental monitoring. T2 - 33. Doktorandenseminar des AK Separation Science CY - Hohenroda, Germany DA - 08.01.2023 KW - Mercury KW - GC/ICP-ToF-MS KW - Isotope dilution PY - 2023 AN - OPUS4-56816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Hoffmann, Katrin A1 - Wegmann, Marc A1 - Hannemann, M. A1 - Somma, V. A1 - Jochum, T. A1 - Niehaus, J. A1 - Roggenbuck, D. T1 - Automated determination of genotoxicity of nanoparticles with DNA-based optical assays - The NANOGENOTOX project N2 - The overall interest in nanotoxicity, triggered by the increasing use of nanomaterials in the material and life sciences, and the synthesis of an ever increasing number of new functional nanoparticles calls for standardized test procedures1,2 and for efficient approaches to screen the potential genotoxicity of these materials. Aiming at the development of fast and easy to use, automated microscopic methods for the determination of the genotoxicity of different types of nanoparticles, we assess the potential of the fluorometric γH2AX assay for this purpose. This assay, which can be run on an automated microscopic detection system, relies on the detection of DNA double strand breaks as a sign for genotoxicity3. Here, we provide first results obtained with broadly used nanomaterials like CdSe/CdS and InP/ZnS quantum dots as well as iron oxide, gold, and polymer particles of different surface chemistry with previously tested colloidal stability and different cell lines like Hep-2 and 8E11 cells, which reveal a dependence of the genotoxicity on the chemical composition as well as the surface chemistry of these nanomaterials. These studies will be also used to establish nanomaterials as positive and negative genotoxicity controls or standards for assay performance validation for users of this fluorometric genotoxicity assay. In the future, after proper validation, this microscopic platform technology will be expanded to other typical toxicity assays. T2 - SPIE 2018 CY - San Francisco, USA DA - 27.01.2018 KW - Nanoparticle KW - Fluorescence KW - Surface chemistry KW - Size KW - Assay KW - Microscopy KW - Nanotoxicity KW - Toxicity KW - Automation KW - Calibration KW - Standard PY - 2018 AN - OPUS4-44186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike A1 - Jung, Christian A1 - Werneburg, Martina A1 - Haase, H. A1 - Koch, Matthias T1 - Non-invasive Cereal Analysis by GC-MS detection of Trichodiene as a Volatile Mycotoxin Biomarker N2 - Due to the increasing consumption of cereals worldwide, the monitoring of growth, storage and processing is becoming more and more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sample drawing and procedures for mycotoxin analysis represent a complex challenge for operators, involving invasive and cost intensive steps. Therefore, new time- and labour-saving mycotoxin control methods including sampling and analysis steps are needed. A possible approach is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples and representing the present mycotoxins. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with over 180 compounds. Due to its non-functionalized sesquiterpene structure, trichodiene has already been quantified using Headspace GC-MS methods (for instance). Thereby, it can possibly be used as a biomarker for trichothecene contamination in foodstuff. However, further investigations are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the exact trichothecene content within samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - 10th World Mycotoxin Forum Conference CY - Amsterdam, The Netherlands DA - 11.03.2018 KW - Trichodiene KW - GC-MS KW - Mycotoxin Biomarker PY - 2018 AN - OPUS4-44509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nutsch, A. A1 - Dill, S. A1 - Kamleitner, I. A1 - Sehorz, A. A1 - Schwarzenberger, M. A1 - Streeck, C. A1 - Beckhoff, B. A1 - Merz, H. A1 - Recknagel, Sebastian T1 - A Methodology to Obtain Traceability and Validation of Calibration Samples for Thin Metal Alloy Layers for X-Ray Fluorescence Tools N2 - Statistic process control as well as process capability demand for calibrated determination of layer thicknesses in various industries, e.g. automotive, aerospace, microelectronics manufacturing. Calibration requires well know and well characterized samples. A calibration laboratory accredited according to DIN EN ISO 17025 has the objective to distribute standards traceable to SI units to industrial laboratories for quality control of manufacturing of various products. Especially, the thickness determination of thin metallic coatings e.g. from galvanic processes or layer deposition using X-Ray Fluorescence can be significantly improved by customized calibration samples. This is essential as the measurement uncertainty directly correlates to the capability performing reliable control of processes with high yield. For calibration laboratories, the validation of results using round robins and the direct comparison to national metrology institutes is a prerequisite to demonstrate the competence to perform calibration services. In this paper a strategy to obtain traceability and validation for thin alloy layers as well as first results are presented. The combined use of the accredited method for determination of mass per area from measurement of mass and area combined with standard free X-Ray Fluorescence as well as chemical analysis of dissolved samples with thin layers is deployed for material systems as NixZn1-x as well as NixP1-x. The obtained results are compared to reference free X-Ray Fluorescence at the BESSY II laboratories of Physikalisch-Technische Bundesanstalt. An excellent agreement of the obtained measured values as mass per unit area and alloy concentrations from the different applied methods within the measurement uncertainty was observed for NixP1-x showing the successful performed traceability of the calibration samples to SI units in combination with a validation of results by national metrology institutes and the round robin approach. T2 - European Conference on X-Ray Spectrometry CY - Ljubljana, Slowenia DA - 24.06.2018 KW - Traceability KW - Thin metal alloy layers KW - X-ray fluorescence PY - 2018 AN - OPUS4-45317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike A1 - Drescher, D. A1 - Büchner, T. A1 - Merk, V. A1 - Kneipp, J. A1 - Jakubowski, Norbert T1 - Studying nanoparticle-cell interaction by LA ICP-MS N2 - The interaction of nanoparticles (NPs) with cells has become a major field of interest, ranging from medical applications to nanotoxicology. Size, shape and surface modification of the NPs determine the uptake rate and pathway into the cells, and therefore impact specific cell components and processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is an established quantitative multi-elemental analysis and mapping technique. In recent years, it was shown that LA-ICP-MS can provide quantitative as well as distribution information of NPs in cell samples. Here LA-ICP-MS was applied for the imaging of individual cells to study the uptake and intracellular processing of metal-containing nanostructures. Additionally, the local distribution of naturally occurring elements in cells like P was measured to indicate cell morphology. The cells were incubated with different types of NPs under varying experimental conditions. For LA analysis, the cells were fixed and dried. Our findings show, that LA-ICP-MS is suitable for the localisation of nanoparticle aggregates within cellular compartments. The studied NPs accumulate in the perinuclear region in the course of intracellular processing, but do not enter the cell nucleus. The uptake efficiency depends strongly on the physicochemical properties of the nanostructures as well as on the incubation conditions like concentration and incubation time. The results demonstrate the potential of LA-ICP-MS providing insight into NP uptake, intracellular distribution and cell-to-cell variation dependent on experimental parameters. T2 - Workshop on Laser Bioimaging Mass Spectrometry CY - Münster, Germany DA - 24.05.2018 KW - Imaging KW - Laser ablation KW - ICP-MS KW - Nanoparticle KW - Cell PY - 2018 AN - OPUS4-45071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Heritage Lecture N2 - After finishing my diploma thesis in plasma physics in 1981, I dreamt of a future in a research lab to develop novel fusion reactors for energy production or to study universal plasmas and their emission in the cosmos. This dream never became real, however I found my first job in a team to build up a new museum dedicated to “Energy”, and this first part of my career was already finished after a year, because the funding was not extended. So, I found immediately a new job as a young scientist in the institute for analytical sciences (originally ISAS: Institute for Plasmachemistry and Applied Spectroscopy) in 1982 to develop novel plasma ion sources for inorganic mass spectrometry. The first source of interest was based on a glow discharge for direct analysis of conducting solids (technically supported by Finnigan MAT, Bremen). Here I adopted the design of the Grimm type discharge for the first time, which was well known in optical emission spectroscopy, and coupled it to a quadrupole mass analyzer. The advantage of this design was that flat craters are produced by sputtering which made this source very powerful for in-depth analysis of technical layers. This then became the topic of my PhD, which was not originally planned, and I had to learn a lot about surface analysis. However, since the first project was too successful we established a small team (in cooperation with Jose Broekaert - an expert in ICP-OES) which started with the development of our own inductively coupled plasma ion source in 1986 coupled to a quadrupole and in 1989 to a sector field mass spectrometer (funded by the Minister of Science and Technology; again in cooperation with Finnigan MAT). The latter device was launched to the market in 1993 as the Element 1. The second decade of my career was still related to instrumental development but mainly of glow discharge sources. In an EU funded project first an automated glow discharge sector field instrument was developed where the Grimm type geometry was combined with a fast flow concept (in cooperation with Volker Hoffmann at IFW in Dresden). This was done in cooperation with VG (which became later a part of Thermo Fisher Scientific together with Finnigan MAT), so that it is not surprising that this concept for the Element GD. This project was later continued in the third phase of my career, again funded by the EU and in cooperation with the group of Alfredo Sanz-Medel (Rosario Pereiro and Jorge Pisonero), to develop a fast flow, but now rf-powered GD ion source in combination with a time-of-flight mass spectrometer, which was later launched to the market commercially by Horiba Jobin Yvon (France) for in-depth profiling of thin layers even of non-conducting materials. In the first decade of my career I started to study already “analytical chemistry” from the scratch because the instruments developed have been applied now for direct analysis of solid materials, technical layers and environmental samples. In case of environmental applications our ICP-MS (the quadrupole and the sector field instrument) was coupled with separation techniques, so that this period of instrumental development was dominated in the second decade by development of high efficiency sample introduction systems in combination with speciation studies of Pt group elements, arsenic, selenium and phosphorus (in DNA and phosphorylated proteins), Ni and Cr. Additionally, we continued with the analysis of solid ceramic materials (Al2O3, SiC, SiN) and ambient air-born particles. At the end of the second decade we complemented our instrumental pool by a collision and reaction cell instrument in cooperation with Micromass and used this instrument for speciation studies of peptides and proteins and demonstrated that by ICP-HEX-MS quantitative proteomics is feasible. Therefore, we more and more focused in the following years on metalloproteins and published a famous paper on “Metallobiomolecules: The basis of life, the challenge of atomic spectroscopy” (together with Luc Moens and Ryszard Lobinski). For detection of metalloproteins we applied typical workflows of biochemistry and proteomics, for which I had to extend my knowledge about biochemistry and proteomics. As a new analytical tool, we used a homemade laser ablation cell for sample introduction of metalloproteins after their separation by gel electrophoresis and extended this work by applying metal-tagging of antibodies for Western blot assays. For this purpose, proteins were separated in SDS-PAGE and electroblotted onto membranes. Specific detection of proteins even not containing any metal could be performed by laser ablation ICP-MS using the metal tagged antibodies for indirect detection. This research was interrupted in 2009 by a movement from ISAS (where atomic spectroscopy was declining) to BAM (the Federal Institute for Materials Research and Testing, Berlin) where this research direction was fostered. The experience we achieved at ISAS in the previously mentioned projects were now used here at BAM in the fourth decade for materials research and the development of a quantitative elemental microscope with cellular resolution. So, at the end of my career I am trying to apply all my knowledge and expertise to develop analytical methods and to apply multimodal spectroscopies to decipher the construction code of the cellular machinery, which is the most precise and complex machinery I have ever seen. If we were able to understand how this machinery works, we can better diagnose and treat a malfunction in case of the development of a disease. Finally, I can conclude that lifelong learning starts before school but does not end at the end of this lecture. It looks like this heritage lecture will be focused on my career only, but this is not the case because some highlights of my career will be used to illustrate a few universal principles: how to have fun, how to find friends and how this all leads to an increase of joy and joy is the basis of new ideas (which must not always be related to your profession) and novel ideas are essential for a successful and satisfying career. So, this heritage lecture wants to answer the most important question of a life which was dedicated to plasma spectrochemistry: 1) Is it possible - at all - to have fun in this research direction? 2) Can we learn already today what we need tomorrow? 3) How can we still realize our scientific dreams of cutting edge research in times of cutting budgets? Which automatically leads to the next question: 4) Is necessity the mother of invention? All questions will be answered! Controversial discussions (for angry or disappointed colleagues) will be stimulated and my visions of future research (for students and postdocs) and instrumental developments (for manufacturer) will be presented. Finally, conclusions will be drawn by the auditorium (everybody) and thanks will be given to Ramon Barnes (by me) already in advance! T2 - 2018 Winter Conference on Plasma Spectrochemistry CY - Amelia Island, FL, USA DA - 08.01.2018 KW - History of the research work of Norbert Jakubowski KW - Glow Discharge Mass Spectrometry KW - Inductively Coupled Plasma Mass Spectrometry KW - Laser Ablation PY - 2018 AN - OPUS4-44461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Heritage Lecture N2 - After finishing my diploma thesis in plasma physics in 1981, I dreamt of a future in a research lab to develop novel fusion reactors for energy production or to study universal plasmas and their emission in the cosmos. This dream never became real, however I found my first job in a team to build up a new museum dedicated to “Energy”, and this first part of my career was already finished after a year, because the funding was not extended. So, I found immediately a new job as a young scientist in the institute for analytical sciences (originally ISAS: Institute for Plasmachemistry and Applied Spectroscopy) in 1982 to develop novel plasma ion sources for inorganic mass spectrometry. The first source of interest was based on a glow discharge for direct analysis of conducting solids (technically supported by Finnigan MAT, Bremen). Here I adopted the design of the Grimm type discharge for the first time, which was well known in optical emission spectroscopy, and coupled it to a quadrupole mass analyzer. The advantage of this design was that flat craters are produced by sputtering which made this source very powerful for in-depth analysis of technical layers. This then became the topic of my PhD, which was not originally planned, and I had to learn a lot about surface analysis. However, since the first project was too successful we established a small team (in cooperation with Jose Broekaert - an expert in ICP-OES) which started with the development of our own inductively coupled plasma ion source in 1986 coupled to a quadrupole and in 1989 to a sector field mass spectrometer (funded by the Minister of Science and Technology; again in cooperation with Finnigan MAT). The latter device was launched to the market in 1993 as the Element 1. The second decade of my career was still related to instrumental development but mainly of glow discharge sources. In an EU funded project first an automated glow discharge sector field instrument was developed where the Grimm type geometry was combined with a fast flow concept (in cooperation with Volker Hoffmann at IFW in Dresden). This was done in cooperation with VG (which became later a part of Thermo Fisher Scientific together with Finnigan MAT), so that it is not surprising that this concept for the Element GD. This project was later continued in the third phase of my career, again funded by the EU and in cooperation with the group of Alfredo Sanz-Medel (Rosario Pereiro and Jorge Pisonero), to develop a fast flow, but now rf-powered GD ion source in combination with a time-of-flight mass spectrometer, which was later launched to the market commercially by Horiba Jobin Yvon (France) for in-depth profiling of thin layers even of non-conducting materials. In the first decade of my career I started to study already “analytical chemistry” from the scratch because the instruments developed have been applied now for direct analysis of solid materials, technical layers and environmental samples. In case of environmental applications our ICP-MS (the quadrupole and the sector field instrument) was coupled with separation techniques, so that this period of instrumental development was dominated in the second decade by development of high efficiency sample introduction systems in combination with speciation studies of Pt group elements, arsenic, selenium and phosphorus (in DNA and phosphorylated proteins), Ni and Cr. Additionally, we continued with the analysis of solid ceramic materials (Al2O3, SiC, SiN) and ambient air-born particles. At the end of the second decade we complemented our instrumental pool by a collision and reaction cell instrument in cooperation with Micromass and used this instrument for speciation studies of peptides and proteins and demonstrated that by ICP-HEX-MS quantitative proteomics is feasible. Therefore, we more and more focused in the following years on metalloproteins and published a famous paper on “Metallobiomolecules: The basis of life, the challenge of atomic spectroscopy” (together with Luc Moens and Ryszard Lobinski). For detection of metalloproteins we applied typical workflows of biochemistry and proteomics, for which I had to extend my knowledge about biochemistry and proteomics. As a new analytical tool, we used a homemade laser ablation cell for sample introduction of metalloproteins after their separation by gel electrophoresis and extended this work by applying metal-tagging of antibodies for Western blot assays. For this purpose, proteins were separated in SDS-PAGE and electroblotted onto membranes. Specific detection of proteins even not containing any metal could be performed by laser ablation ICP-MS using the metal tagged antibodies for indirect detection. This research was interrupted in 2009 by a movement from ISAS (where atomic spectroscopy was declining) to BAM (the Federal Institute for Materials Research and Testing, Berlin) where this research direction was fostered. The experience we achieved at ISAS in the previously mentioned projects were now used here at BAM in the fourth decade for materials research and the development of a quantitative elemental microscope with cellular resolution. So, at the end of my career I am trying to apply all my knowledge and expertise to develop analytical methods and to apply multimodal spectroscopies to decipher the construction code of the cellular machinery, which is the most precise and complex machinery I have ever seen. If we were able to understand how this machinery works, we can better diagnose and treat a malfunction in case of the development of a disease. Finally, I can conclude that lifelong learning starts before school but does not end at the end of this lecture. It looks like this heritage lecture will be focused on my career only, but this is not the case because some highlights of my career will be used to illustrate a few universal principles: how to have fun, how to find friends and how this all leads to an increase of joy and joy is the basis of new ideas (which must not always be related to your profession) and novel ideas are essential for a successful and satisfying career. So, this heritage lecture wants to answer the most important question of a life which was dedicated to plasma spectrochemistry: 1) Is it possible - at all - to have fun in this research direction? 2) Can we learn already today what we need tomorrow? 3) How can we still realize our scientific dreams of cutting edge research in times of cutting budgets? Which automatically leads to the next question: 4) Is necessity the mother of invention? All questions will be answered! Controversial discussions (for angry or disappointed colleagues) will be stimulated and my visions of future research (for students and postdocs) and instrumental developments (for manufacturer) will be presented. Finally, conclusions will be drawn by the auditorium (everybody) and thanks will be given to Ramon Barnes (by me) already in advance! T2 - BAM-Doktorandenseminar CY - Berlin, Germany DA - 07.02.2018 KW - History of the research work of Norbert Jakubowski KW - Glow Discharge Mass Spectrometry KW - Inductively Coupled Plasma Mass Spectrometry KW - Laser Ablation PY - 2018 AN - OPUS4-44462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia A1 - Koch, Matthias A1 - Haase, H. T1 - Kopplung von Elektrochemie und Massenspektrometrie in der Mykotoxinforschung N2 - Mykotoxine werden als sekundäre Metabolite von Schimmelpilzen gebildet und haben diverse schädliche Effekte auf Menschen, Tiere und Pflanzen. Laut FAO sind weltweit bis zu 25 % aller Lebens- und Futtermittel mit Mykotoxinen kontaminiert, wodurch jährlich immense ökonomische Verluste entstehen. Neben den eigentlichen Mykotoxinen rücken zunehmend deren Transformationsprodukte (TPs) in den Fokus. Diese können als natürliche Stoffwechselprodukte toxischer sein als das eigentliche Mykotoxin und stellen eine potenzielle zusätzliche Gefahr für den Verbraucher dar. TPs werden überwiegend mit in vitro und in vivo Techniken untersucht, welche sowohl zeit- als auch kostenintensiv sind. Ziel war es nun, schnelle und zudem verlässliche Techniken zur Simulation von TPs diverser Mykotoxine zu testen. Die Kopplung von Elektrochemie und Massenspektrometrie, kurz EC/MS, als rein instrumenteller Ansatz 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/MS, EC/LC/MS und HPLC-MS Techniken (MS/MS und FT-ICR) wurden nun die Mykotoxine Zearalenon, Citrinin und Dihydroergocristin (als Modellsubstanz für die Ergotalkaloide) elektrochemisch bei Potentialen bis zu 2500 mV vs. Pd/H2 oxidiert und deren TPs mit mikrosomalen in vitro Ansätzen verglichen. Hierbei konnten mehrere Übereinstimmungen hydroxylierter Spezies, sowohl elektrochemisch als auch biochemisch generiert, festgestellt werden. Die EC/MS ist somit auch in der Lebensmittelanalytik als nützliches und vielseitiges Werkzeug verwendbar. T2 - 24. Arbeitstagung des Regionalverband Nordost der LChG CY - Berlin, Germany DA - 06.03.2018 KW - Elektrochemie KW - Mykotoxine KW - Metabolismus PY - 2018 AN - OPUS4-44425 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Rosner, M. A1 - Tütken, T. T1 - Exploring variations in the three-isotope space: A new approach and application to magnesium isotope fractionation in the mammal food web N2 - In chemical elements with three or more stable isotopes, mass-dependent stable isotope fractionation is expressed by co-varying isotope ratios. In the three-isotope space ((δ’m2/δ’m1)/(( δ’m3/δ’m1)) these plot along a line with a slope (β), the so called ‘terrestrial fractionation line’. This partitioning of stable isotopes results from both kinetic and equilibrium reactions that are characterized by specific β-values. For the natural range of isotope ratios of ‘novel’ stable isotope systems such as Si, Mg, Fe, Zn, Cu this information cannot be accessed because samples fall close to the delta-zero standard where the current measurement precision is too low to resolve small differences in β. We present a new approach to resolve deviations from a reference slope β by standard-sample bracketing against material offset from the natural range. We use this approach to explore the isotope fractionation mechanism in the mammalian food web. We have analyzed Mg stable isotope ratios in bone bioapatite of herbivore, omnivore and carnivore mammals. Positive shifts in δ26/24Mg along the trophic chain (from herbivore to carnivore) together with β= 0.513 suggest the presence of two isotope fractionation mechanisms operating during biomineralization. While positive shifts in δ26/24Mg are in favor of equilibrium isotope fractionation process, the proximity of β to the theoretically calculated β(kinetic) of typically 0.511 suggests the presence of a second component that fractionates stable isotopes kinetically. The herein presented approach is applicable to any element with 3+ stable isotopes analyzed by multi-collector inductively coupled plasma mass spectrometry. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Magnesium delta values KW - Equilibrium isotope fractionation KW - Kinetic isotope fractionation KW - Measurement uncertainty KW - Mammals KW - Food web PY - 2018 AN - OPUS4-44643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike A1 - Drescher, D. A1 - Büchner, T. A1 - Pisonero, J. A1 - Bouzas-Ramos, D. A1 - Kneipp, J. A1 - Jakubowski, Norbert T1 - LA-ICP-MS to study nanoparticle-cell interaction N2 - Nanoparticles (NPs) have found a wide range of applications in research and industry. Thereby the interaction of NPs with biological systems like cells has become a major field of interest, ranging from medical applications to nanotoxicology. Size, shape and surface modification of the nanomaterials determine the uptake rate and pathway into the cells, and therefore impact specific cell components and processes. In recent years, elemental imaging of biological samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining more and more importance. Improvements concerning both spatial resolution (down to 1 µm) and signal-to-background ratio due to low-dispersion LA chambers make LA-ICP-MS particularly interesting for single cell analysis. Here LA-ICP-MS was applied for the imaging of individual cells to study the uptake and intracellular processing of metal-containing nanostructures. The cells were incubated with different NPs under varying experimental conditions and afterwards fixed with para-formaldehyde and dried for LA analysis. High-spatial resolution LA-ICP-MS was achieved by careful optimisation of the laser ablation parameters. Our findings show, that LA-ICP-MS is applicable to localize NP aggregates within cellular compartments. The uptake efficiency depends strongly on the physicochemical properties of the nanostructures as well as on the incubation conditions like concentration and incubation time. The results demonstrate the potential of LA-ICP-MS providing insight into nanoparticle-cell interaction dependent on experimental parameters. T2 - 14th European Workshop on Laser Ablation (EWLA) CY - Pau, France DA - 26.06.2018 KW - Laser ablation KW - ICP-MS KW - Imaging KW - Nanoparticle KW - Cell PY - 2018 AN - OPUS4-45570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mansurova, Maria A1 - Bell, Jérémy A1 - Gotor, Raul A1 - Rurack, Knut T1 - Fluorescence-based optical system for the detection of total petroleum hydrocarbons in water and soil with smartphone read-out compatibility - Spectrocube, a sensor for rapid oil test in water and soil N2 - Contamination of natural bodies of water with oil and lubricants (or generally, hydrocarbon derivatives such as petrol, fuel and others) is a commonly found phenomenon around the world due to the extensive production, transfer and use of fossil fuels. The timely identification of these contaminants is of utmost importance, since they directly affect water quality and represent a risk for wildlife and human health even in trace amounts. In this work, we develop a simple system for the on-field detection of total petroleum hydrocarbons (TPH) in water and soil, the "Spectrocube". The test is based on the measurement of the fluorescence signal emitted by the molecular rotor 4-DNS-OH dye. This dye is embedded in a hydrophobic polymeric matrix (PVDF), avoiding interactions of water with the dye and providing a robust support for use in test-strip fashion. The test-strip’s fluorescence intensity increases linearly at low concentrations of TPH, reaching a saturation value at higher concentrations. For excitation and evaluation of the test-strip fluorescence, a simple miniature optical system was designed. The system works semi-quantitatively as solvent-free TPH detection kit, as well as quantitatively when using a simple cyclopentane extraction step. To simplify the fluorescence read-out, the device is coupled to a tablet computer via Bluetooth, running a self-programmed software ("app"). T2 - Oil Spill India 2018 CY - New Delhi, India DA - 05.07.2018 KW - Oil analysis KW - Water analysis KW - Fluorescence KW - Spectrocube KW - Rapid test KW - Field test KW - Spectroscopy KW - Sensor PY - 2018 AN - OPUS4-45606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert A1 - Müller, L. A1 - Wanka, Antje T1 - Development of immuno-assays and metal-staining techniques for bioimaging of cells and tissues using LA-ICP-MS N2 - We are using LA-ICP-MS to quantify metals in biological cells and thin cuts of tissues from varies organs. Different applications will be presented to demonstrate the state of the art of bioimaging to visualize the elemental distribution pattern in soft bio-materials (tissue, single cells) of metals, metal containing stains and metal-tagged antibodies. For this purpose, different strategies for metal tagging will be presented and will be compared in terms of analytical figures of merit. First applications for detection of biomarkers in animal and human tissue samples will be presented. In a first example, we have applied LA-ICP-MS to visualize the local distribution of proteins, which are used as bio-markers for neurodegenerative diseases. For this purpose, brain tissues from mice experiments have been stained by metal-tagged antibodies. House-keeping proteins have been investigated as internal cellular standards. Additionally, ink-jet printing of metal doped inks onto the surface of tissue samples has been applied for drift corrections and quantification. Validation of our results are achieved in comparison to immune-histochemical staining and optical microscopy. In a second example, we used specific metal-tagged antibodies for detection of biomarker specific for prostate cancer. For this purpose, micro tissue arrays are incubated with metal-tagged antibodies for bioimaging of samples from many patients using simultaneous detection of all relevant biomarkers and their tags. For improvement of sensitivity in the next example application nanoparticle tagged antibodies for detection of metallothionines in eye lens tissue samples will be discussed. Recently we have used our tagging and staining strategies to determine the cell cycle of single cells, which is of future interest for toxicological studies. Finally, future trends in elemental microscopy and mass cytometry imaging will be discussed. T2 - Workshop on Laser Bioimaging Mass Spectrometry CY - Münster, Germany DA - 24.05.2018 KW - Single cell analysis KW - LA-ICP-MS KW - Immuno-Assays PY - 2018 AN - OPUS4-45160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia A1 - Borzekowski, Antje A1 - Haase, H. A1 - Rueß, L. A1 - Menzel, R. A1 - Koch, Matthias T1 - Using the model organism Caenorhabditis elegans for the toxicity testing of citrinin, zearalenone and zearalenone-14-sulfate N2 - To keep up with emerging mycotoxins and their transformation products fast and reliable toxicity tests are needed. Toxicity testing of mycotoxins is carried out usually by performing in vitro assays or is evaluated by using laboratory animals like mice, rats or chicken in in vivo studies. Settled between classical in vitro approaches and in vivo studies with higher animals are tests with the nematode Caenorhabditis elegans. Since Sydney Brenner described 1974 the cultivation and handling of C. elegans, this worm is widely used as model organism in developmental biology and neurology. Due to many benefits like easy and cheap cultivation, a completely sequenced genome and short generation time, it also plays an important role in toxicological research. Finally, the high number of conserved genes between human and C. elegans make the worm an ideal candidate for toxicological investigations. In this study we used C. elegans to assess the toxic effects of the relevant food mycotoxin citrinin (CIT), the mycoestrogen zearalenone (ZEN) and the modified mycotoxin ZEN-14-sulfate (ZEN-14-S) on different lifetable parameters including reproduction, thermal and oxidative stress tolerance and lifespan. All tested mycotoxins significantly decreased the amount of offspring. In case of ZEN and CIT also significant negative effects on stress tolerance and lifespan were observed compared to the control group. Moreover, metabolization of mycotoxins in the worms was investigated by using LC MS/MS. Extraction of the worms treated 5 days with mycotoxin-containing and UVC-killed bacteria showed metabolization of ZEN to α-ZEL and β-ZEL (ZEL = zearalenol, ratio about 3:2). ZEN 14-S was reduced to ZEL 14-S and CIT was metabolized to mono hydroxylated CIT. T2 - 40th Mycotoxin Workshop CY - Munich, Germany DA - 11.06.2018 KW - Mycotoxins KW - Caenorhabditis elegans KW - Toxicity testing PY - 2018 AN - OPUS4-45170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - 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 - CONF A1 - Gornushkin, Igor B. T1 - Laser induced Plasma: Modeling and diagnostics N2 - Laser-induced plasmas are widely used in many areas of science and technology; examples include spectrochemical analysis, thin film deposition, material processing, and even jet propulsion. Several topics will be addressed. First, general phenomenology of laser-induced plasmas will be discussed. Then, a chemical model will be presented based on a coupled solution of Navier-Stokes, state, radiative transfer, material transport, and chemical (Guldberg-Waage) equations. Results of computer simulations for several chemical systems will be shown and compared to experimental observations obtained by optical imaging, spectroscopy, and tomography. The latter diagnostic tools will also be briefly discussed. T2 - Lecture at the Dept of Chemistry of Czeged University (Hungary) on 31.05.2019 CY - Czeged, Hungary DA - 31.05.2019 KW - Plasma KW - LIBS KW - Plasma modeling PY - 2019 AN - OPUS4-48188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Several approaches to calibration-free LIBS: Advantages and pitfalls N2 - An overview of calibration-free laser induced breakdown spectroscopy (CF LIBS) methods is presented. Advantages and pitfalls of these methods are critically discussed. T2 - Workshop of the Spectrochemical Working Committee (SWC) of the Hungarian Academy of Sciences CY - Budapest, Hungary DA - 05.06.2019 KW - Calibration-free LIBS KW - CF LIBS algorithms PY - 2019 AN - OPUS4-48189 LA - eng 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 - Faßbender, Sebastian A1 - Rodiouchkina, K. A1 - Vanhaecke, F. A1 - Meermann, Björn T1 - On-line species-specific isotopic analysis of sulfur by hyphenation of capillary electrophoresis with MC-ICP-MS N2 - In many scientific fields, isotopic analysis can offer valuable information. 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. Whereas some works hyphenating GC and IC with MC-ICP-MS have already been reported, LC and CE hyphenations are still inadequately represented based on the capabilities of these separation techniques. 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 using a multiple-injection approach for instrumental mass bias correction by standard-sample bracketing. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared to data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was promising regarding the differentiation of the river systems by the isotopic signature of river water sulfate. The great potential of this method is based on the versatility of the applied separation technique, not only in the environmental field but also for, e.g., biomolecules, as sulfur is the only covalently bound constituent of proteins that can be analyzed by MC-ICP-MS. T2 - Virtual Goldschmidt 2020 CY - Online meeting DA - 21.06.2020 KW - Isotopic analysis KW - Hyphenated techniques KW - Capillary electrophoresis KW - Multicollector-ICP-MS KW - Speciation analysis PY - 2020 AN - OPUS4-50922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Von der Au, Marcus A1 - Borovinskaya, O. A1 - Büchel, C. T1 - Metal based pollutant assessment via diatoms - new possibilities via automated single cell-ICP-ToF-MS N2 - Diatoms are located at the bottom of the food chain. Toxicological relevant metals can possibly accumulate within the food web and cause harmful effects. Diatoms are a test system in ecotoxicology. Toxicological effects weaken the growth of algae which is by default investigated by means of fluorescence detection. On basis of the expose concentration as well as obtained fluorescence data potential threshold exceedance in e.g. surface waters is assessed. However, this approach does not allow for the determination of “real” accumulated metal concentration in diatoms. Common approaches are based on bulk analysis via e.g. ICP-MS, ICP-OES or AAS. But, biological variability is completely disregarded. To tackle this problem, alternative approaches are highly needed. Within the last years, sp-ICP-MS for nanoparticle as well as single cell analysis turned out as a powerful technique to analyze metal contents as well as size distributions on broad size range. But, common ICP-MS systems do not allow for multi-element detection within single particle/cell events. Thus, simultaneous MS detection devices are needed - just recently, ICP-ToF-MS experienced a revival. Within our previous work, we developed an automated sample introduction system based on a HPLC system on-line with single particle-ICP-MS, which allowed for ionic background separation and single algae analysis. However, for unambiguous tracing several fingerprint elements and multielement analysis in single algae (diatoms) is needed. Thus, we coupled our previous setup on-line to ICP-ToF-MS. Test diatom species were exposed to test substances (Zn) as well as nanoparticles (FeNPs). The developed setup allowed for a fast, automated and multielement analysis in single diatoms. Furthermore, we combined our approach with multivariate data assessment - multielement detection of characteristic fingerprint elements allowed for an unambiguous diatom tracing. Clustering of diatoms according to metal exposure concentration levels was enabled. Our approach is a new potential tool in ecotoxicological testing. T2 - 53. DGMS & 27th ICP-MS user meeting CY - Münster, Germany DA - 01.03.2020 KW - Single cell-ICP-ToF-MS KW - Diatoms KW - New ecotoxicological testing tools PY - 2020 AN - OPUS4-50644 LA - eng 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 - 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 - 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 - 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 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - Capillary electrophoresis KW - Hyphenated techniques KW - Isotopic analysis KW - Multicollector-ICP-MS KW - Speciation analysis PY - 2020 AN - OPUS4-50501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus A1 - Metzger, M. A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - HR-CS-GF-MAS as a new screening method for emerging pollutants - per- and polyfluorinated substances in the environment N2 - The introduction of fluorine in organic molecules leads to new chemical/physical properties. Especially in the field of pharmaceuticals, fluorinated organic molecules are becoming more and more popular and at present amount up to 25% of market share, with an upward trend. The main benefits of fluorinated pharmaceuticals are: (i) enhanced fat solubility; (ii) enhanced interaction of catalytic-center of enzymes with fluorine-drugs; (iii) a delayed metabolism within the human body. Highly fluorinated organic substances are also used in technical applications (e.g. coatings, fire-extinguishing agents). Due to the broad variety of fluorinated substances and increasing production volumes numerous and up to date unknown fluorine-species are most likely to be present in the (aquatic) environment. Analytical methods to assess the degree of contamination of surface waters with organically bound fluorine are highly needed and up to now only combustion ion chromatography based method is available, which is relatively laborious. Since a few years’ high resolution-continuum source-graphite furnace atomic absorption spectrometers (HR-CS-GFAAS) are commercially available from Analytik Jena. By means of this technique, the detection of high resolution molecular absorption spectra (MAS) is enabled. Thus, fluoride is detectable upon the addition of a modifier and the formation of a diatomic molecule (e.g. GaF). Just recently, we applied this technique for total fluorine (mainly dissolved fluoride) analysis in river water samples. In the present work a HR-CS-GFMAS method for extractable organically bound fluorine (EOF) analysis in surface water samples was developed by us. The method is based on SPE extraction of organically bound fluorine even in the presence of high fluoride concentrations followed by HR-CS-GFMAS analysis upon elution. Due to high enrichment factors, LODs in the low ng/L range were achieved. We successfully applied our SPE HR-CS-GFMAS method to Rhine water samples and EOF in the range of about 50-300 ng/L was detectable. T2 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - SPE HR-CS GF MAS PY - 2020 AN - OPUS4-50504 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 - 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 - 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 - 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 - 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 - Radtke, Martin A1 - Berger, Achim T1 - Tragbare RFA an Gläsern: Ergebnisse und Grenzen N2 - Vorstellung der Ergebnisse der Messungen an Gläsern von Goethes Prismen. T2 - 3. Goethe/Ritter-Workshop CY - Berlin, Germany DA - 25.05.2018 KW - Goethe KW - Farbenlehre KW - Prisma KW - Handheld KW - XRF PY - 2018 AN - OPUS4-46369 LA - deu 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 - Gornushkin, Igor B. T1 - Plasma fundamentals and diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, microreactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basics of plasma computer modeling will be presented. T2 - 03.-06. September 2018, 13 Symposium "Massenspektrometrische Verfahren der Elementspurenanalyze", BAM, Berlin, Adlershof CY - BAM, Berlin, Adlershof, Germany DA - 03.09.2018 KW - Thermal equilibrium KW - Plasma processes KW - Electron number density KW - Temperatures KW - Emission line profiles KW - Spatial information KW - Plasma modeling PY - 2018 AN - OPUS4-46108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. T1 - Dynamical chemical model of laser induced plasma N2 - Laser induced plasma (LIP) is a highly dynamic, short living event which presents significant difficulty for both diagnostics and modeling. The former requires precise spatially- and time-resolved measurements on a micron-nanosecond scale while the latter needs numerous descriptive parameters; many of them can only be obtained from experiment. Diagnostics and modeling should always complement each other for obtaining a truthful picture of LIP. In this presentation, a newly developed collisional-dominated model will be presented. The model is based on the coupled Navier-Stokes, state, radiative transfer, material transport, and chemical equations. The model incorporates plasma chemistry through the equilibrium approach that relies on atomic and molecular partition functions. Several chemical systems are modeled including Si-C-Cl-N and B-H-Cl systems. The model is used to study the equilibrium states of the systems as functions of the concentrations of plasma species and plasma temperature. The model also predicts the evolution of number densities of atomic and molecular species in the expanding plasma plume. T2 - 18.09.2018, 9th International Conference on PLASMA PHYSICS AND PLASMA TECHNOLOGY (PPPT‐9) CY - Minsk, Belorussia DA - 17.09.2018 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2018 AN - OPUS4-46111 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 - Resch-Genger, Ute A1 - Würth, Christian A1 - Geissler, Daniel A1 - Weigert, Florian A1 - Kaiser, Martin T1 - Spectroscopic characterization of semiconductor and lanthanide-based nanocrystals with vis and NIR emission N2 - Common approaches to improve the optical properties of semiconductor quantum dots and lanthanide doped nanophosphors present core/shell structures as radiationless deactivation at the particle surface is usually the main energy loss mechanism. This has led to increasingly sophisticated particle architectures using multishell systems with shells of different chemical composition and thickness and initiated an increasing number of quantitative spectroscopic studies focusing on the key performance parameter photoluminescence quantum yield to identify optimum particle structures. This is particularly challenging in the long wavelength region > 1000 nm and for nonlinear emitters like upconversion nanocrystals. Here, we present suitable absolute methods to quantify the photoluminescence of these different emitters in the vis/NIR/IR and as function of excitation power density and underline the impact of such measurements on a profound mechanistic understanding of the nonradiative deactivation pathways in semiconductor and upconversion nanocrystals of different size and particle architecture in different environments. T2 - NANO 2018 CY - Hong Kong, People's Republic of China DA - 24.06.2018 KW - Upconversion KW - Semiconductor KW - Quantum dot KW - Nanoparticle KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Surface chemistry KW - Deactivation pathways KW - Modeling KW - Size PY - 2018 AN - OPUS4-45797 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 - Gornushkin, Igor B. A1 - Sergei, S. A1 - Kornev, R.A. A1 - Sennikov, P. G. T1 - Equilibrium chemistry of boron halides in plasma chemical reactors N2 - High purity halides of III-VI group elements, especially chloride and fluorides, are used in gas phase technologies for obtaining high purity materials and coatings. The reduction of halides in hydrogen-halide mixtures can be achieved in various discharge plasmas, e.g. inductively coupled, ark, and even laser-induced plasmas. Existing models of such plasmas are not sufficiently accurate to predict a yield of the targeted compounds and to describe the plasma processes involved in formation of these compounds. Besides, a construction of costly plasma-chemical reactors can be alleviated by the prior modeling of plasma processes that may occur in such reactors. A goal of this work is to extend the model, which was initially developed for laser induced Plasmas, to plasmas used in chemical reactors, in particular, the inductively-coupled-RF discharge Plasma. The model predicts equilibrium chemical compositions of reaction mixtures as functions of plasma temperature and stoichiometry of reactants. The mixtures investigated are BCl3/H2/Ar and BF3/H2/Ar where Ar serves as the plasma-forming gas and H2 as a binding agent which binds the active species Cl and F and Cl- and F-containing intermediates to produce gaseous B and its condensate. An additional goal is to obtain information about intermediate reaction products for different ratios of BCl3/H2 and BF3/H2 and at different temperatures and different Ar flow rates. It is found that the desired components B and B2 appear at appreciable concentrations of >0.1% and ~0.01% respectively only at temperatures above 3000 K. It is also established that the effect of charged species on the reaction products is miniscule for temperatures below 5000 K. The expected yield of boron as a function of the original mole fraction H2/BCl3 and H2/BF3 is calculated. The mole fractions are varied in the range 0.1-1000 and the temperature in the range 1000-10000 K. It is shown that the yield of boron increases with increasing the molar ratio H2/BCl3 and H2/BF3 up to ~100 in the temperature range 2000-5000 K. At higher temperatures, T>5000 K, the boron concentration reaches its maximum and does not depend on the concentration of hydrogen; all molecules dissociate and chemical reactions proceed only between charged particles (mostly elemental ions) and electrons. The calculated plasma parameters and composition are compared with experimental data obtained by optical emission spectroscopy. The calculated plasma temperature and electron density are shown to be in good agreement with the measured ones. T2 - European Winter Conference on Plasma Spectrochemistry (EWSPS-2019) CY - Pau, France DA - 03.02.2019 KW - Chemical reactors KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2019 AN - OPUS4-47541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. T1 - Modeling chemistry in laser-induced and other types of plasmas N2 - A goal of this work is to extend the model, which was initially developed for laser induced plasmas, to plasmas used in chemical reactors, in particular, the inductively-coupled-RF discharge plasma. The model predicts equilibrium chemical compositions of reaction mixtures as functions of plasma temperature and stoichiometry of reactants. The mixtures investigated are BCl3/H2/Ar and BF3/H2/Ar where Ar serves as the plasma-forming gas and H2 as a binding agent which binds the active species Cl and F and Cl- and F-containing intermediates to produce gaseous B and its condensate. An additional goal is to obtain information about intermediate reaction products for different ratios of BCl3/H2 and BF3/H2 and at different temperatures and different Ar flow rates. It is found that the desired components B and B2 appear at appreciable concentrations of >0.1% and ~0.01% respectively only at temperatures above 3000 K. It is also established that the effect of charged species on the reaction products is miniscule for temperatures below 5000 K. The expected yield of boron as a function of the original mole fraction H2/BCl3 and H2/BF3 is calculated. The mole fractions are varied in the range 0.1-1000 and the temperature in the range 1000-10000 K. It is shown that the yield of boron increases with increasing the molar ratio H2/BCl3 and H2/BF3 up to ~100 in the temperature range 2000-5000 K. At higher temperatures, T>5000 K, the boron concentration reaches its maximum and does not depend on the concentration of hydrogen; all molecules dissociate and chemical reactions proceed only between charged particles (mostly elemental ions) and electrons. The calculated plasma parameters and composition are compared with experimental data obtained by optical emission spectroscopy. The calculated plasma temperature and electron density are shown to be in good agreement with the measured ones. T2 - Workshop on Laser and Plasmas Applications CY - Bari, Italy DA - 04.03.2019 KW - Plasma KW - LIBS KW - Plasma modeling PY - 2019 AN - OPUS4-47545 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 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben. T2 - Jahrestagung des GDMB-Chemiker-Ausschusses CY - Kassel, Germany DA - 07.11.2023 KW - Referenzmaterial KW - Messunsicherheit KW - ISO Guide 35 PY - 2023 AN - OPUS4-58929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben. T2 - 11. VDI-Fachtagung Messunsicherheit und Prüfprozesse CY - Erfurt, Germany DA - 14.11.2023 KW - Referenzmaterial KW - Messunsicherheit KW - ISO Guide 35 PY - 2023 AN - OPUS4-58946 LA - deu 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 -