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 - Piechotta, Christian A1 - Kovačič, A. A1 - Steinhäuser, Lorin A1 - Heath, E. A1 - Lardy-Fontan, S. T1 - A method for monitoring estrogens in whole surface waters by GC-MS/MS N2 - Natural and synthetic estrogens are key endocrine-disrupting chemicals. Despite occurring at ultra-trace levels (below ng L-1), it is believed that they are contributing to an increase in feminized fish and other endocrine disruptive effects, and hence, their inclusion in the Watch list was not unexpected. One of the main sources ofestrogens to surface waters is wastewater effluent. Once in surface waters, they can partition into different compartments, i.e., water and suspended particulate matter. For this reason, there is an urgent need for a methodology to monitor estrogen levels below the environmental quality standards (EQS) set by the Water Framework Directive requirements. In this study, a precise and accurate gas chromatography-mass spectrometry method (GC-MS/MS) for the analysis of estrone (E1), 17β-estradiol (17β-E2), 17α-estradiol (17α- E2), 17-alpha-ethinylestradiol (EE2), and estriol (E3) in whole water samples with ng L-1 limit of quantification (LOQ) was developed and validated in accordance with CEN/TS 16800:2020 guidelines. T2 - IMSC 2022 CY - Maastricht, Netherlands DA - 27.08.2022 KW - EDC KW - WFD KW - GC-MS PY - 2022 AN - OPUS4-57097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - A Long Way of Plasma Modeling: Personal Experience N2 - Modeling is an important tool for understanding a physical phenomenon. It helps to interpret results of experiments and optimize experimental parameters for obtaining a desirable result. Modeling laser induced plasma is beneficial for many scientific and industrial fields, e.g., analytical chemistry, pulsed laser deposition, plasma enhanced chemical vapor deposition, laser welding, additive manufacturing etc. In this presentation, a personal experience in development of a physical model of laser induced plasma will be given in a chronological sequence starting from early 2000th and until now. Over the time, the model evolved from its simple analytical form that described plasma emission spectra to its current numerical form that describes plasma dynamics, chemistry, and interaction with a substrate surface. Several examples will be given for the application of the model to practical problems such as spectroscopic chemical analysis, plasma enhanced chemical vapor deposition, and surface modification by laser ablation. T2 - XII World Conference on Laser Induced Breakdown Spectroscopy CY - Bari, Italy DA - 05.09.2022 KW - Laser induced plasma KW - CFD computational fluid dynamic KW - Plasma modeling KW - Plasma chemistry PY - 2022 AN - OPUS4-55669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bosc-Bierne, Gaby T1 - A generic, cost-efficient HPLC-HRMS method for quality control of peptide pools N2 - Synthetic peptide pools are used in antigen-specific T-cell assays, which are an important part in vaccine and immunotherapeutic clinical trials. As the analytical characterization is challenging due to the similarity of the single peptides or is expensive due to isotope labeled standards, usually only a pre-characterization of the single peptides is performed. However, a regular quality control of the peptide mix would be highly desirable. Therefore, a cost-efficient high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) method for quality control of a model peptide pool is developed. Peptides were synthesized using peptides&elephants proprietary libraries of individual peptides (LIPS) technology and purified by reversed-phase chromatography to > 90% each. The lyophilized single peptides were combined to a model peptide pool and analyzed by reversed-phase high-performance capillary liquid chromatography coupled to an orbitrap mass spectrometer. Separation was performed on a capillary reversed phase column (2 μm, ID x L 300 μm x 150 mm) with a linear gradient of acetonitrile + 0,05% trifluoroacetic acid. After optimizing the injection mode, the gradient elution, the temperature and the additives a model peptide pool was separated. The extracted ion chromatogram (XIC) was studied to confirm the exact masses. By combination of capillary HPLC and HRMS a new cost-efficient quality control method could be developed for the separation and identification of complex synthetic peptide pools. T2 - 5th European Congress of Immunology CY - Amsterdam, The Netherlands DA - 02.09.2018 KW - Peptide pools KW - Quality control KW - LC-MS PY - 2018 AN - OPUS4-45858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, M. A. A1 - Khan, I. A1 - Opitz, P. A1 - Hartmann, J: A1 - Ashraf, M. A1 - Qurashi, A. A1 - Prädel, L. A1 - Panthöfer, M. A1 - Cossmer, Antje A1 - Pfeifer, Jens A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Meermann, Björn A1 - Mondeshki, M. A1 - Tahir, M. N. A1 - Tremel, W. T1 - A Generalized Method for High-Speed Fluorination of Metal Oxides by Spark Plasma Sintering Yields Ta3O7F and TaO2F with High Photocatalytic Activity for Oxygen Evolution from Water N2 - A general method to carry out the fluorination of metal oxides with poly(tetrafluoroethylene) (PTFE, Teflon) waste by spark plasma sintering (SPS) on a minute scale with Teflon is reported. The potential of this new approach is highlighted by the following results. i) The tantalum oxyfluorides Ta3O7F and TaO2F are obtained from plastic scrap without using toxic or caustic chemicals for fluorination. ii) Short reaction times (minutes rather than days) reduce the process time the energy costs by almost three orders of magnitude. iii) The oxyfluorides Ta3O7F and TaO2F are produced in gram amounts of nanoparticles. Their synthesis can be upscaled to the kg range with industrial sintering equipment. iv) SPS processing changes the catalytic properties: while conventionally prepared Ta3O7F and TaO2F show little catalytic activity, SPS-prepared Ta3O7F and TaO2F exhibit high activity for photocatalytic oxygen evolution, reaching photoconversion efficiencies up to 24.7% and applied bias to photoconversion values of 0.86%. This study shows that the materials properties are dictated by the processing which poses new challenges to understand and predict the underlying factors. KW - Fluorination KW - Oxygen evolution reaction KW - Photocatalysis KW - Spark plasma sintering KW - Tantalum oxyfluorides PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524329 DO - https://doi.org/10.1002/adma.202007434 VL - 23 IS - 20 SP - 7434 PB - Wiley‐VCH GmbH AN - OPUS4-52432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Langenhan, Jennifer A1 - Jaeger, Carsten A1 - Baum, K. A1 - Simon, M. A1 - Lisec, Jan T1 - A Flexible Tool to Correct Superimposed Mass Isotopologue Distributions in GC‐APCI‐MS Flux Experiments N2 - The investigation of metabolic fluxes and metabolite distributions within cells by means of tracer molecules is a valuable tool to unravel the complexity of biological systems. Technological advances in mass spectrometry (MS) technology such as atmospheric pressure chemical ionization (APCI) coupled with high resolution (HR), not only allows for highly sensitive analyses but also broadens the usefulness of tracer‐based experiments, as interesting signals can be annotated de novo when not yet present in a compound library. However, several effects in the APCI ion source, i.e., fragmentation and rearrangement, lead to superimposed mass isotopologue distributions (MID) within the mass spectra, which need to be corrected during data evaluation as they will impair enrichment calculation otherwise. Here, we present and evaluate a novel software tool to automatically perform such corrections. We discuss the different effects, explain the implemented algorithm, and show its application on several experimental datasets. This adjustable tool is available as an R package from CRAN. KW - Mass Spectrometry KW - Isotopologue Distribution KW - Metabolic Flux KW - R package PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547318 DO - https://doi.org/10.3390/metabo12050408 VL - 12 IS - 5 SP - 1 EP - 10 PB - MDPI AN - OPUS4-54731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raysyan, Anna T1 - A fast dipstick immunoassay for the determination of DCF in the breast milk N2 - Diclofenac (DCF) is a non-steroidal anti-inflammatory drug (NSAID) with analgetic, anti-inflammatory, and antipyretic properties. The mechanism of action of diclofenac, like that of other NSAIDs, involves inhibition of cyclooxygenase (COX-1 and COX-2). Another pharmacological effect is preventing of prostaglandin synthesis in vitro. Prostaglandins are mediators of inflammation, because diclofenac is an inhibitor of prostaglandin synthesis. A method has been developed to analyse for diclofenac (DCF) in the milk. T2 - BIONNALE Speed Lecture Award 2018 CY - Berlin, Germany DA - 20.06.2018 KW - Milk KW - DCF KW - Immunoassay PY - 2018 AN - OPUS4-46753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - von der Au, Marcus A1 - Wittwer, Phillip A1 - Roesch, Philipp A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Meermann, Björn T1 - A fast and simple PFAS extraction method utilizing HR–CS–GFMAS for soil samples N2 - Here, we describe an optimized fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) in soils utilizing high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR–CS–GFMAS). To omit the bias of the solid phase extraction (SPE) step commonly used during the analysis of extractable organically bound fluorine (EOF) we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol without any additional SPE. Four extraction steps were representative to determine a high proportion of the EOF (>80% of eight extractions). Comparison of the optimized method with and without an additional SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. Differences of up to 94% were observed which were not explainable by coextracted inorganic fluoride. Therefore, not only a more accurate but also a more economic as well as ecologic method (bypassing of unnecessary SPE) was developed. The procedural limit of quantification (LOQ) of the developed method was 10.30 μg/kg which was sufficient for quantifying EOF concentrations in all tested samples. For future PFAS monitoring and potential regulative decisions the herein presented optimized extraction method can offer a valuable contribution. KW - Per- and polyfluorinated alkly substances (PFASs) KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Soils KW - Solid phase extraction (SPE) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction PY - 2022 DO - https://doi.org/10.1016/j.chemosphere.2022.133922 VL - 295 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-54359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - von der Au, Marcus A1 - Meermann, Björn T1 - A fast and simple PFAS extraction method for soil samples utilizing HR-CS-GFMAS 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 - SALSA Make and Measure ... and Machines CY - Online meeting DA - 16.09.2021 KW - PFAS KW - HR-CS-GFMAS KW - IC KW - EOF KW - Soil PY - 2021 AN - OPUS4-53302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - A fast and simple PFAS extraction method for soil sample analysis using HR-CS-GFMAS N2 - Per- and polyfluorinated alkyl substances (PFASs) are a substance class of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their different chemical and physical properties as well as the high number of target substances. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate a realistic PFAS pollution level. PFAS sum parameters compromise the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for indirect fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we describe a fast and simple extraction method for the determination of the EOF using HR-CS-GFMAS in soil samples. Common approaches for the EOF determination use solid phase extraction (SPE). To omit the bias of this time consuming and expensive step we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol. Comparison of the method with and without an SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. In the next step, the applicability of our method was tested for other solid matrices. In view of steadily increasing numbers of PFASs, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFASs in the future. T2 - Analytica conference CY - München, Germany DA - 21.06.2022 KW - PFAS KW - HR-CS-GFMAS KW - Soil KW - Fluorine KW - SPE PY - 2022 AN - OPUS4-55124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -