TY - JOUR A1 - Thinnes, A. A1 - Westenberger, M. A1 - Piechotta, Christian A1 - Letho, L. A1 - Wirth, F. A1 - Lau, H. A1 - Klein, J. T1 - Cholinergic and metabolic effects of metformin in mouse brain N2 - Metformin is widely used as a first-line treatment for type 2 diabetes, but central effects of metformin have received little attention. When metformin (200 mg/kg i.p.) was administered to C57Bl6 mice, metformin concentration in cerebrospinal fluid peaked at 29 μM after 30 min but dropped quickly and was low at 90 min. In mouse hypothalamus sampled by microdialysis, systemically administered metformin caused minor and transient increases of acetylcholine, glucose and lactate while choline levels decreased. When metformin (0.2−10 mM) was locally infused via retrodialysis, there was a short-lasting increase of acetylcholine in the hypothalamus. Extracellular lactate levels in hypothalamus showed a massive increase upon metformin infusion while glucose levels decreased. In isolated mitochondria of mouse brain, metformin inhibited oxygen consumption and the activity of complex I. Inhibition of mitochondrial respiration likely explains lactate formation in the brain during metformin infusion which may cause lactic acidosis during metformin intoxication. The changes of cholinergic activity in the hypothalamus may be associated with appetite suppression observed during metformin treatment. KW - Metformin KW - Blood-brain barrier KW - Lactate KW - Glucose KW - Microdialysis KW - Hypothalamus PY - 2021 DO - https://doi.org/10.1016/j.brainresbull.2021.02.018 SN - 0361-9230 VL - 170 SP - 211 EP - 217 PB - Elsevier CY - Amsterdam, Niederlande AN - OPUS4-52189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Chips or strips – the importance of embedding and integration in (bio)chemical assay development N2 - The most important aspect of developing a miniaturized or compact (bio)chemical assay for use outside a dedicated laboratory environment is, of course, the design of the recognition and signaling element that best achieves the required selectivity and sensitivity in relation to the target analyte and analytical scenario. For luminescence assays, this essentially means that the appropriate combination of small-molecule binding units, ligands or biomacromolecular binders such as antibodies or aptamers and organic, metal-organic or rare earth metal ion luminophores or luminescent nanoparticles such as semiconductor nanocrystals, carbon nanodots, polymer dots or fluorescently doped silica or polymer nanoparticles as well as the best strategy for combining binding and signaling unit must be selected. Having accomplished this task and obtained first promising results in a conventional laboratory setting with the use of pipettes, cuvettes and benchtop spectrometers, the challenge is to bridge the gap between such a model assay and an assay that uses a mobile and robust device in the hands of a layperson and does not require complicated operation and extensive manual steps, especially when handling liquids, at best in line with the ASSURED principle, being affordable, sensitive, specific, user-friendly, rapid and robust, equipment free and deliverable to end-users, or, as recently proposed, the REASSURED principle, which furthermore includes real-time connectivity and ease of specimen collection (translating into ease of sampling in the non-diagnostic world). In order to close this gap, it is of utmost importance to know the further requirements of the assay, i.e., whether only one or more than one analyte needs to be detected, what the main potential interferents are and how tolerant the assay is to the sample matrix, as well as how many assays are typically performed per hour/day/week, how long a run should take and how expensive a single analysis should be. These parameters usually determine the most appropriate format, i.e., whether it is a dip stick, a test strip, a lateral flow assay, a microfluidic chip, a 3D-microfluidic approach or a combination thereof, in conjunction with a dedicated readout system or a mobile communication device. This choice in turn determines the most appropriate strategy for integration, i.e., whether the recognition and signaling element are used directly in liquid solution,8 embedded in polymer layers or gels, attached to surfaces of planar substrates, micro- or nanoparticles or immobilized or loaded in micro- or nanoparticles, which could then enable direct or controlled/gated access. This contribution discusses various aspects of this multi-stage process using examples from the group. T2 - How to develop a sensor? Academic Approaches vs. Industrial Interests (EU Training School) CY - Kaiserslautern, Germany DA - 18.09.2024 KW - Sensing KW - Rapid testing KW - Microfluidics KW - Test strips KW - Device integration PY - 2024 AN - OPUS4-61429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, M. A1 - Frings, P. J. A1 - Oelze, Marcus A1 - Herwartz, D. A1 - Lünsdorf, K. A1 - Wiedenbeck, M. T1 - Chert oxygen isotope ratios are driven by Earth's thermal evolution N2 - The 18O/16O ratio of cherts (δ18Ochert) increases nearly monotonically by ~15‰ from the Archean to present. Two end-member explanations have emerged: cooling seawater temperature (TSW) and increasing seawater δ18O (δ18Osw). Yet despite decades of work, there is no consensus, leading some to view the δ18Ochert record as pervasively altered. Here, we demonstrate that cherts are a robust archive of diagenetic temperatures, despite metamorphism and exposure to meteoric fluids, and show that the timing and temperature of quartz precipitation and thus δ18Ochert are determined by the kinetics of silica diagenesis. A diagenetic model shows that δ18Ochert is influenced by heat flow through the sediment column. Heat flow has decreased over time as planetary heat is dissipated, and reasonable Archean-modern heat flow changes account for ~5‰ of the increase in δ18Ochert, obviating the need for extreme TSW or δ18Osw reconstructions. The seawater oxygen isotope budget is also influenced by solid Earth cooling, with a recent reconstruction placing Archean δ18OSW 5 to 10‰ lower than today. Together, this provides an internally consistent view of the δ18Ochert record as driven by solid Earth cooling over billion-year timescales that is compatible with Precambrian glaciations and biological. KW - Climate KW - Oxygen isotope ratios KW - Silica diagenesis KW - Early Earth KW - Heat flow PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569359 DO - https://doi.org/10.1073/pnas.2213076119 SN - 0027-8424 VL - 119 IS - 51 SP - 1 EP - 7 PB - National Academy of Sciences CY - Washington, DC AN - OPUS4-56935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Chemometrical analysis of spectral data obtained from glow discharge optical emission spectroscopy for elemental analysis of metals N2 - The poster shows the combination of GD-OES and machine learning. The gola of this project is to establish a new and robust calibration model, which can be used to identify elemental composition and concentration of metals from a single spectra. T2 - Salsa make and measure Konferenz CY - Online meeting DA - 16.09.2021 KW - Glow discharge optical emission spectroscopy KW - Machine learning PY - 2021 AN - OPUS4-53323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tannenberg, Robert A1 - Paul, Martin A1 - Röder, Bettina A1 - Gande, S. L. A1 - Sreeramulu, S. A1 - Saxena, K. A1 - Richter, C. A1 - Schwalbe, H. A1 - Swart, C. A1 - Weller, Michael G. T1 - Chemiluminescence biosensor for the determination of cardiac troponin I (cTnI) N2 - Cardiac troponin I (cTnI) is a crucial biomarker for diagnosing cardiac vascular diseases, including acute myocardial infarction (AMI). This study presents a proof-of-concept chemiluminescence-based immunosensor for rapid and accurate measurement of cTnI, with the potential for online monitoring. The immunosensor incorporates a flow cell design and a sensitive complementary metal-oxide-semiconductor (CMOS) camera for optical readout. A microfluidic setup was established to enable selective and quasi-online determination of cTnI within ten minutes. The sensor was tested with recombinant cTnI in phosphate buffer, demonstrating measurements in the concentration range of 2–25 µg/L, with a limit of detection (LoD) of 0.6 µg/L (23 pmol/L) achieved using the optimized system. The immunosensor exhibited high selectivity, as no cross-reactivity was observed with other recombinant proteins such as cTnT and cTnC at a concentration of 16 µg/L. Measurements with diluted blood plasma and serum yielded an LoD of 60 µg/L (2.4 nmol/L) and 70 µg/L (2.9 nmol/L), respectively. This biosensor offers a promising approach for the rapid and sensitive detection of cTnI, contributing to the diagnosis and management of acute myocardial infarction and other cardiac vascular diseases. N2 - Das kardiale Troponin I (cTnI) ist ein wichtiger Biomarker für die Diagnose von Herz-Kreislauf-Erkrankungen, einschließlich des akuten Myokardinfarkts (AMI). In dieser Studie wird ein auf Chemilumineszenz basierender Immunsensor für die schnelle und genaue Messung von cTnI vorgestellt, der das Potenzial für eine Online-Überwachung hat. Der Immunsensor besteht aus einer Durchflusszelle und einer empfindlichen CMOS-Kamera (Complementary Metal-Oxide-Semiconductor) zur optischen Detektion. Es wurde ein mikrofluidischer Aufbau entwickelt, der eine selektive und quasi Online-Bestimmung von cTnI innerhalb von zehn Minuten ermöglicht. Der Sensor wurde mit rekombinantem cTnI in Phosphatpuffer getestet und zeigte einen Messbereich von 2-25 µg/L, wobei mit dem optimierten System eine Nachweisgrenze (LoD) von 0,6 µg/L (23 pmol/L) erreicht wurde. Der Immunsensor zeigte eine hohe Selektivität, da keine Kreuzreaktivität mit anderen rekombinanten Proteinen wie cTnT und cTnC bei einer Konzentration von 16 µg/L beobachtet wurde. Messungen mit verdünntem Blutplasma und Serum ergaben einen LoD von 60 µg/L (2,4 nmol/L) bzw. 70 µg/L (2,9 nmol/L). Dieser Biosensor bietet einen vielversprechenden Ansatz für den schnellen und empfindlichen Nachweis von cTnI, der zur Diagnose und Behandlung des akuten Myokardinfarkts und anderer kardialer Gefäßerkrankungen beitragen kann. KW - Acute myocardial infarction KW - Heart attack KW - Emergency KW - Diagnosis KW - Cardiac troponin KW - Biomarker KW - Immunosensor KW - Biosensor KW - Chemiluminescence KW - Luminol KW - Peroxidase KW - Monoclonal antibodies KW - Flow injection immunoassay KW - Immunometric assay KW - Immunometric biosensor KW - Microfluidic system KW - Monolithic column KW - Online biosensor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575471 DO - https://doi.org/10.3390/bios13040455 SN - 2079-6374 VL - 13 IS - 4 SP - 1 EP - 20 PB - MDPI CY - Basel AN - OPUS4-57547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziegler, K. A1 - Kunert, A. T. A1 - Reinmuth-Selzle, K. A1 - Leifke, A. L. A1 - Widera, D. A1 - Weller, Michael G. A1 - Schuppan, D. A1 - Fröhlich-Nowoisky, J. A1 - Lucas, K. A1 - Pöschl, U. T1 - Chemical modification of pro-inflammatory proteins by peroxynitrite increases activation of TLR4 and NF-κB: Implications for the health effects of air pollution and oxidative stress N2 - Environmental pollutants like fine particulate matter can cause adverse health effects through oxidative stress and inflammation. Reactive oxygen and nitrogen species (ROS/RNS) such as peroxynitrite can chemically modify proteins, but the effects of such modifications on the immune system and human health are not well understood. In the course of inflammatory processes, the Toll-like receptor 4 (TLR4) can sense damage-associated molecular patterns (DAMPs). Here, we investigate how the TLR4 response and pro-inflammatory potential of the proteinous DAMPs α-Synuclein (α-Syn), heat shock protein 60 (HSP60), and high-mobility-group box 1 protein (HMGB1), which are relevant in neurodegenerative and cardiovascular diseases, changes upon chemical modification with peroxynitrite. For the peroxynitrite-modified proteins, we found a strongly enhanced activation of TLR4 and the pro-inflammatory transcription factor NF-κB in stable reporter cell lines as well as increased mRNA expression and secretion of the pro-inflammatory cytokines TNF-α, IL-1β, and IL-8 in human monocytes (THP-1). This enhanced activation of innate immunity via TLR4 is mediated by covalent chemical modifications of the studied DAMPs. Our results show that proteinous DAMPs modified by peroxynitrite more potently amplify inflammation via TLR4 activation than the native DAMPs, and provide first evidence that such modifications can directly enhance innate immune responses via a defined receptor. These findings suggest that environmental pollutants and related ROS/RNS may play a role in promoting acute and chronic inflammatory disorders by structurally modifying the body's own DAMPs. This may have important consequences for chronic neurodegenerative, cardiovascular or gastrointestinal diseases that are prevalent in modern societies, and calls for action, to improve air quality and climate in the Anthropocene. KW - Protein nitration KW - Protein oligomerization KW - Damage-associated molecular patterns (DAMPs) KW - Pattern recognition receptor KW - Anthropocene KW - Environmental pollutants PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517128 DO - https://doi.org/10.1016/j.redox.2020.101581 VL - 37 SP - 101581 PB - Elsevier B.V. AN - OPUS4-51712 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Chemical characterization of aging processes in high energy-density lithium-ion batteries N2 - Introduction Lithium-ion batteries (LIBs) are one key technology to overcome the climate crisis and energy transition challenges. Demands of electric vehicles on higher capacity and power drives research on innovative cathode and anode materials. These high energy-density LIBs are operated at higher voltages, leading to increased electrolyte decay and the current collectors' degradation. Even though this fundamental corrosion process significantly affects battery performance, insufficient research is being done on the aluminum current collector. Fast and convenient analytical methods are needed for monitoring the aging processes in LIBs. Methods In this work glow-discharge optical emission spectrometry (GD-OES) was used for depth profile analysis of aged cathode material. The measurements were performed in pulsed radio frequency mode. Under soft and controlled plasma conditions, high-resolution local determination (in depth) of the elemental composition is possible. Scanning electron microscopy (SEM) combined with a focused ion beam (FIB) cutting and energy dispersive X-ray spectroscopy (EDX) was used to confirm GD-OES results and obtain additional information on elemental distribution. Results The aging of coin cells manufactured with different cathode materials (LCO, LMO, NMC111, NMC424, NMC532, NMC622, and NMC811) was studied. GD-OES depth profiling of new and aged cathode materials was performed. Quantitative analysis was possible through calibration with synthetic standards and correction by sputter rate. Different amounts of aluminum deposit on the cathode surface were found for different materials. The deposit has its origin in the corrosion of the aluminum current collector. The results are compatible with results from FIB-EDX. However, GD-OES is a faster and less laborious analytical method. Therefore, it will accelerate research on corrosion processes in high energy-density batteries. Innovative aspects - Quantitative depth profiling of cathode material -Monitoring of corrosion processes in high energy-density lithium-ion batteries - Systematic investigation of the influence of different cathode materials T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Lithium Ion Batteries KW - GD-OES KW - Depth-profiling PY - 2023 AN - OPUS4-58586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Avci, Fatma T1 - Characterization of black mass by X-Ray fluorescence spectroscopy N2 - X-ray fluorescence analysis (XRF) is a method of elemental analysis that is used either as wavelength dispersive XRF (WDXRF) or energy dispersive XRF (EDXRF). Using EDXRF, it is possible to analyze samples within a few minutes without time-consuming sample preparation. This makes the method potentially suitable for analyzing larger sample quantities under industrial conditions. However, the XRF method is matrix-dependent. Depending on the cathode material of the recycled batteries, there are significant differences in the composition of the resulting black mass. This means that specific calibration models must be developed for different types of black mass. The aim of our work is to use the EDXRF method to reliably analyze black mass of different origins with regard to the elements that are particularly interesting for recycling: nickel (Ni), manganese (Mn), cobalt (Co), aluminum (Al), iron (Fe), zinc (Zn), silicon (Si), copper (Cu), and phosphorus (P). Based on the different mass fractions of the elements mentioned, black masses from used lithium-ion batteries can be divided into three groups according to the cathode chemistry: lithium nickel manganese cobalt oxide (NMC), lithium cobalt oxide (LCO), and mixed chemistries (MC), the latter of which may contain lithium iron phosphate (LFP). The division into groups is necessary to determine the matrices and thus select the appropriate calibration model for the analysis of the EDXRF data in order to achieve the most accurate determination of the elemental content possible. Reference analyses are performed using WDXRF. The score plots obtained by PLS-DA of the specific elemental composition of the black masses examined to date by both WDXRF and EDXRF reveal a correct separation of the BM matrix types LCO, NMC, and MC. Our preliminary results with test samples yielded 100 % correct predictions with both data sets. However, only two matrix types, NMC and LCO, have been tested with the EDXRF data so far. Data for MC is pending as work progresses. T2 - Doctoral seminar 2025 - Working Group Chemometrics and Quality Assurance (GDCh) CY - Hamburg, Germany DA - 11.09.2025 KW - Black Mass KW - XRF Spectroscopy KW - Chemometric Modeling KW - PLS-DA PY - 2025 AN - OPUS4-64095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chan, George C.-Y. A1 - Engelhard, Carsten A1 - Wiley, Joshua S. A1 - Shoulds, Ayanna U. A1 - Cooks, R. Graham A1 - Hieftje, Gary M. A1 - Shelley, Jacob T. T1 - Characterization of a Low-Temperature Plasma (LTP) Ambient Ionization Source Using Temporally Resolved Monochromatic Imaging Spectrometry N2 - The low-temperature plasma (LTP) probe is a common plasma-based source used for ambient desorption–ionization mass spectrometry (MS). While the LTP probe has been characterized in detail with MS, relatively few studies have used optical spectroscopy. In this paper, two-dimensional (2D) imaging at selected wavelengths is used to visualize important species in the LTP plasma jet. First, 2D steady-state images of the LTP plume for N2+ (391.2 nm), He I (706.5 nm), and N2 (337.1 nm) emissions were recorded under selected plasma conditions. Second, time-resolved 2D emission maps of radiative species in the LTP plasma jet were recorded through the use of a 200 ns detection gate and varying gate delays with respect to the LTP trigger pulse. Emission from He I, N2+, and N2 in the plasma jet region was found to show a transient behavior (often referred to as plasma bullets) lasting only a few microseconds. The N2+ and He I maps were highly correlated in spatial and temporal structure. Further, emission from N2 showed two maxima in time, one before and one after the maximum emission for N2+ and He I, due to an initial electronic excitation wave and ion–electron recombination, respectively. Third, the interaction of the LTP probe with a sample substrate and an electrically grounded metallic needle was studied. Emission from a fluorophore on the sample substrate showed an initial photon-induced excitation from plasma-generated photons followed by electronic excitation by other plasma species. The presence of a grounded needle near the plasma jet significantly extended the plasma jet lifetime and also generated a long-lived corona discharge on the needle. The effect of LTP operating parameters on emission spectra was correlated with mass-spectral results including reagent-ion signals. Lastly, five movies provide a side-by-side comparison of the temporal behavior of emitting species and insights into the interactions of the emission clouds with a sample surface as well as an external needle. Temporally and spatially resolved imaging provided insights into important processes in the LTP plasma jet, which will help improve analyte ion sampling in LTP–MS. KW - Optical spectroscopy KW - Low-temperature plasma KW - Ambient ionization KW - Instrumentation PY - 2023 DO - https://doi.org/10.1177/00037028231184501 VL - 77 IS - 8 SP - 940 EP - 956 PB - SAGE Publications AN - OPUS4-61269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Characterization and quantification of functional groups and coatings on nanoobjects an overview N2 - Characterization of Nanoparticles – Questions to Ask, Functional Nanoparticles (NPs) – Organic, Inorganic, and Hybrid Nanoparticles Nanomaterial Characterization Standardization – Addressing Remaining Gaps Surface FGs Particle Surface Chemistry - Why is it Important? Particle Surface Chemistry - A Key Driver for Performance, Applications, and Safety Aspects Method Development for Quantifying FGs and Ligands on Particle Surfaces FG Quantification – Method Choice & Criteria Relevant for Data Interpretation Quantifying the Amount of Total and Accessible FGs on Aminated Silica Nanoparticles (SiO2-NH2) Comparing the Total and Accessible –NH2 Content on Aminated Silica NPs of Different Size Characterization of Nanoparticles Standardization Standardized Measurements of Surface FGs on Nanoparticles EMP Project SMURFnano EMP Project SMURFnano Work Packages & Goals Certified Reference Materials from BAM T2 - e-MRS 2024 (Spring Meeting of the European Materials Research Society, Altech Symposium) CY - Strasbourg, France DA - 27.05.2024 KW - Luminescence KW - Nano KW - Particle KW - Quantum yield KW - Quality assurance KW - Interlaboratory comparison KW - Method KW - Uncertainty KW - Reference material KW - Surface analysis KW - Optical assay KW - NMR KW - Silica KW - Ligand PY - 2024 AN - OPUS4-60495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kazlagić, Anera A1 - Rosner, M. A1 - Cipriani, A. A1 - Frick, D. A. A1 - Glodny, J. A1 - Hoffmann, E. J. A1 - Hora, J. M. A1 - Irrgeher, J. A1 - Lugli, F. A1 - Magna, T. A1 - Meisel, T. C. A1 - Meixner, A. A1 - Possolo, A. A1 - Pramann, A. A1 - Pribil, M. J. A1 - Prohaska, T. A1 - Retzmann, Anika A1 - Rienitz, O. A1 - Rutherford, D. A1 - Paula-Santos, G. M. A1 - Tatzel, M. A1 - Widhalm, S. A1 - Willbold, M. A1 - Zuliani, T. A1 - Vogl, Jochen T1 - Characterisation of conventional 87Sr/86Sr isotope ratios in cement, limestone and slate reference materials based on an interlaboratory comparison study N2 - An interlaboratory comparison (ILC)was organised to characterise 87Sr/86Sr isotope ratios in geological and industrial reference materials by applying the so-called conventional method for determining 87Sr/86Sr isotope ratios. Four cements (VDZ 100a,VDZ 200a, VDZ 300a, IAG OPC-1), one limestone (IAG CGL ML-3) and one slate (IAG OU-6) reference materials were selected, covering a wide range of naturally occurring Sr isotopic signatures. Thirteen laboratories received aliquots of these six reference materials together with a detailed technical protocol. The consensus values for the six reference materials and their associated measurement uncertainties were obtained by applying a Gaussian, linear mixed effects model fitted to all the measurement results. By combining the consensus values and their uncertainties with an uncertainty contribution for potential heterogeneity, reference values ranging from 0.708134 mol mol-1 to 0.729778 mol mol-1 were obtained with relative expanded uncertainties of ≤ 0.007 %. This study represents an ILC on conventional 87Sr/86Sr isotope ratios, within which metrological principles were considered and the compatibility of measurement results obtained by MC-ICP-MS and by MC-TIMS is demonstrated. The materials characterised in this study can be used as reference materials for validation and quality control purposes and to estimate measurement uncertainties in conventional 87Sr/86Sr isotope ratio measurement. KW - Sr isotope analysis KW - Isotope ratios KW - Cement KW - Geological material KW - MC-TIMS KW - MC-ICP-MS KW - Interlaboratory comparison KW - Measurement uncertainty KW - Cconventional method PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579836 DO - https://doi.org/10.1111/ggr.12517 SN - 1639-4488 VL - 47 IS - 4 SP - 821 EP - 840 PB - Wiley online library AN - OPUS4-57983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Lisec, Jan A1 - Koch, Matthias T1 - Changes in Black Truffle (Tuber melanosporum) Aroma during Storage under Different Conditions N2 - The enticing aroma of truffles is a key factor for their culinary value. Although all truffle species tend to be pricy, the most intensely aromatic species are the most sought after. Research into the aroma of truffles encompasses various disciplines including chemistry, biology, and sensory science. This study focusses on the chemical composition of the aroma of black truffles (Tuber melanosporum) and the changes occurring under different storage conditions. For this, truffle samples were stored under different treatments, at different temperatures, and measured over a total storage time of 12 days. Measurements of the truffle aroma profiles were taken with SPME/GC–MS at regular intervals. To handle the ample data collected, a systematic approach utilizing multivariate data analysis techniques was taken. This approach led to a vast amount of data which we made publicly available for future exploration. Results reveal the complexity of aroma changes, with 695 compounds identified, highlighting the need for a comprehensive understanding. Principal component analyses offer initial insights into truffle composition, while individual compounds may serve as markers for age (formic acid, 1-methylpropyl ester), freshness (2-Methyl-1-propanal; 1-(methylthio)-propane), freezing (tetrahydrofuran), salt treatment (1-chloropentane), or heat exposure (4-hydroxy-3-methyl-2-butanone). This research suggests that heat treatment or salt contact significantly affects truffle aroma, while freezing and cutting have less pronounced effects in comparison. The enrichment of compounds showing significant changes during storage was investigated with a metabolomic pathway analysis. The involvement of some of the enriched compounds on the pyruvate/glycolysis and sulfur pathways was shown. KW - Mass Spectrometry KW - Metabolomics KW - Tuber melanosporum KW - Truffle Aroma PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601731 DO - https://doi.org/10.3390/jof10050354 VL - 10 IS - 5 SP - 1 EP - 22 PB - MDPI AN - OPUS4-60173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klein, Luise A1 - Wilke, Olaf T1 - Chamber comparison for the determination of initial VOC emissions from consumer products N2 - Volatile organic compound (VOC) emissions from consumer products contribute to human inhalation exposure and may cause adverse health effects. Existing methods to determine long-term VOC emissions from e.g. building products need to be verified for their suitability to reliably detect initial VOC emissions from consumer products within the first hours and days of use, which would facilitate realistic inhalation exposure assessments. To investigate this issue, VOCs emitted from a test sample were determined in a large-scale emission test chamber and in two micro-chambers of different volumes, and the results were compared. T2 - Healthy Buildings 2023 Europe CY - Aachen, Germany DA - 11.06.2023 KW - Micro-chamber KW - Emission test chamber KW - Volatile organic compounds KW - Inhalation exposure KW - Consumer products PY - 2023 SP - 6 EP - 8 AN - OPUS4-58055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Michael G. T1 - Challenges of protein analysis N2 - Selected Projects BAM Division 1.5 Test for sensitive SARS-CoV-2 detection Corundum as a novel affinity support Troponin biosensor based on chemiluminescence Plant virus purification (CCMV) Protein Quantification by 1H-NMR Ultra-miniaturized Biosensors N2 - Ausgewählte Projekte BAM-Abteilung 1.5 Test für empfindlichen SARS-CoV-2-Nachweis Korund als neuartige Affinitätscarriermaterialien Troponin-Biosensor auf Basis von Chemilumineszenz Reinigung von Pflanzenviren (CCMV) Proteinquantifizierung durch 1H-NMR Ultra-miniaturisierte Biosensoren T2 - Klausurtagung der MPI Abteilung „Multiphasenchemie“ CY - Mainz, Germany DA - 19.11.2024 KW - Corona test KW - Corundum KW - Affinity separation KW - Affinity chromatography KW - Troponin biosensor KW - Peptide aptamer KW - Cowpea chlorotic mottle virus KW - Nanoparticle KW - Nanocarrier KW - Nuclear magnetic resonance NMR KW - Protein quantification KW - HyPhox KW - Ring resonator PY - 2024 AN - OPUS4-62126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Sarah A1 - Konthur, Zoltán A1 - Weller, Michael G. A1 - Jaeger, Carsten A1 - Reinders, Yvonne T1 - Challenges and Insights in Absolute Quantification of Recombinant Therapeutic Antibodies by Mass Spectrometry: An Introductory Review N2 - This review describes mass spectrometry (MS)-based approaches for the absolute quantification of therapeutic monoclonal antibodies (mAbs), focusing on technical challenges in sample treatment and calibration. Therapeutic mAbs are crucial for treating cancer and inflammatory, infectious, and autoimmune diseases. We trace their development from hybridoma technology and the first murine mAbs in 1975 to today’s chimeric and fully human mAbs. With increasing commercial relevance, the absolute quantification of mAbs, traceable to an international standard system of units (SI units), has attracted attention from science, industry, and national metrology institutes (NMIs). Quantification of proteotypic peptides after enzymatic digestion using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has emerged as the most viable strategy, though methods targeting intact mAbs are still being explored. We review peptide-based quantification, focusing on critical experimental steps like denaturation, reduction, alkylation, choice of digestion enzyme, and selection of signature peptides. Challenges in amino acid analysis (AAA) for quantifying pure mAbs and peptide calibrators, along with software tools for targeted MS data analysis, are also discussed. Short explanations within each chapter provide newcomers with an overview of the field’s challenges. We conclude that, despite recent progress, further efforts are needed to overcome the many technical hurdles along the quantification workflow and discuss the prospects of developing standardized protocols and certified reference materials (CRMs) for this goal. We also suggest future applications of newer technologies for absolute mAb quantification. KW - Monoclonal antibody KW - Therapeutic antibodies KW - Mass spectrometry KW - Liquid chromatography KW - Absolute quantification KW - Metrology KW - Traceability KW - Certified reference material PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623707 DO - https://doi.org/10.3390/antib14010003 SN - 2073-4468 VL - 14 IS - 1 SP - 1 EP - 26 PB - MDPI CY - Basel, Schweiz AN - OPUS4-62370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Döring, Sarah A1 - Weller, Michael G. A1 - Reinders, Yvonne A1 - Konthur, Zoltán A1 - Jaeger, Carsten T1 - Challenges and Insights in Absolute Quantification of Recombinant Therapeutic Antibodies by Mass Spectrometry: An Introductory Review N2 - This review describes mass spectrometry (MS)-based approaches for the absolute quantification of therapeutic monoclonal antibodies (mAbs), focusing on technical challenges in sample treatment and calibration. Therapeutic mAbs are crucial for treating cancer, inflammatory, infectious, and autoimmune diseases. We trace their development from hybridoma technology and the first murine mAbs in 1975 to today’s chimeric and fully human mAbs. With increasing commercial relevance, absolute quantification of mAbs, traceable to SI units, has attracted attention from science, industry, and national metrology institutes (NMIs). Quantification of proteotypic peptides after enzymatic digestion using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has emerged as the most viable strategy, though methods targeting intact mAbs are still being explored. We review peptide-based quantification, focusing on critical experimental steps like denaturation, reduction, alkylation, choice of digestion enzyme, and selection of signature peptides. Challenges in amino acid analysis (AAA) for quantifying pure mAbs and peptide calibrators, along with software tools for targeted MS data analysis, are also discussed. Short explanations within each chapter provide newcomers an overview of the field’s challenges. Finally, we discuss prospects and limitations of developing standardized protocols and certified reference materials (CRMs) and suggest future applications of newer technologies for the absolute quantification of therapeutic antibodies. KW - Antibody KW - Mass spectrometry KW - Absolute quantification KW - Metrology KW - Reference products PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621841 DO - https://doi.org/10.20944/preprints202412.1081.v1 SP - 1 EP - 22 PB - MDPI AN - OPUS4-62184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Güttler, Arne T1 - Certified Reference Materials for the Quantification and Standardization of Fluorescence-based Measurements N2 - The size and shape of photoluminescence signals is affected by wavelength-, polarization-, and time-dependent instrumentspecific contributions and the compound- and environment-specific photoluminescence quantum yield. The former hamper the comparability of fluorescence measurements performed on different measuring devices. The commonly relatively done determination of the performance parameter requires suitable quantum yield standards with well-known. The performance of such measurements is, e.g., described in the written standard IEC 62607 currently revised. T2 - Colloquium für Optische Spektrometrie 2025 CY - Jena, Germany DA - 24.09.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Advanced material KW - Calibration KW - Characterization KW - Fluorescence quantum yield KW - Phosphor KW - Absolute KW - Integrating sphere spectroscopy KW - Dye KW - Standardization KW - Reference material KW - Interlaboratory comparison KW - Uncertainty PY - 2025 AN - OPUS4-64213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Recknagel, Sebastian T1 - Certified reference materials for the determination of cadmium (Cd) in cocoa N2 - BAM has produced three cocoa CRMs certified for cadmium (ERM-BD513 – 515) as tools for checking analytical methods for Cd-determination. KW - Certified reference material KW - Cocoa KW - Cadmium PY - 2021 SP - 4 EP - 4 AN - OPUS4-53694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation, analysis and certification of a new certified glass reference material (CRM) for the determination of hydrolytic resistance of borosilicate glass with the glass grains test is described. The CRM BAM-S053 is available in the form of glass rods (length: 185 mm, diameter: 9 mm, weight: 27·5 g). Certified properties are the acid consumption determined according to the procedures described in ISO 720, USP<660>, Ph.Eur. 3.2.1, data obtained following the procedure of ISO 719 was scattering too widely. The certified values are based on the results of 15 laboratories which participated in the certification interlaboratory comparison. The CRM is intended for the quality control when applying ISO 720, USP<660>, Ph.Eur. 3.2.1 and with limitations ISO 719. KW - CRM KW - Hydrolytic resistance KW - Borosilicate glass PY - 2021 DO - https://doi.org/10.13036/17533562.62.1.001 VL - 62 IS - 1 SP - 25 EP - 27 AN - OPUS4-52195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation of certified reference material for the determination of hydrolytic resistance of borosilicate glass is described. Certified properties are the acid consumption according to the relevant standard procedures described in ISO 720, USP<660> and Ph.Eur. 3.2.1. T2 - 26. International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Borosilicate glass KW - CRM KW - Hydrolytic resistance PY - 2022 AN - OPUS4-55521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Isleyen, Alper A1 - Can, Suleyman Z. A1 - Cankur, Oktay A1 - Engin, Betul Ari A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Horvat, Milena A1 - Jacimovic, Radojko A1 - Zuliani, Tea A1 - Fajon, Vesna A1 - Jotanovic, Aida A1 - Gaževic, Luka A1 - Milosevic, Milena A1 - Ochsenkuehn–Petropoulou, Maria A1 - Tsopelas, Fotis A1 - Lymberopoulou, Theopisti A1 - Tsakanika, Lamprini-Areti A1 - Serifi, Olga A1 - Ochsenkuehn, Klaus M. A1 - Bulska, Ewa A1 - Tomiak, Anna A1 - Kurek, Eliza A1 - Cakılbahçe, Zehra A1 - Aktas, Gokhan A1 - Altuntas, Hatice A1 - Basaran, Elif A1 - Kısacık, Barıs A1 - Gumus, Zeynep T1 - Certification of the total element mass fractions in UME EnvCRM 03 soil sample via a joint research project N2 - Soil certified reference material (CRM), UME EnvCRM 03 was produced by a collaborative approach among national metrology institutes, designated institutes and university research laboratories within the scope of the EMPIR project: Matrix Reference Materials for Environmental Analysis. This paper presents the sampling and processing methodology, homogeneity, stability, characterization campaign, the assignment of property values and their associated uncertainties in compliance with ISO 17034:2016. The material processing methodology involves blending a natural soil sample with a contaminated soil sample obtained by spiking elemental solutions for 8 elements (Cd, Co, Cu, Hg, Ni, Pb, Sb and Zn) to reach the level of warning risk monitoring values specified for metals and metalloids of soils in Europe. Comparative homogeneity and stability test data were obtained by two different institutes, ensuring the reliability and back up of the data. The certified values and associated expanded uncertainties for the total mass fractions of thirteen elements (As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, V and Zn) are established. The developed CRM can be used for the development and validation of measurement procedures for the determination of the total mass fractions of elements in soil and also for quality control/assurance purposes. The developed CRM is the first example of a soil material originating from Türkiye. KW - Total element content KW - Soil KW - CRM KW - Certification KW - Environmental pollution monitoring PY - 2024 DO - https://doi.org/10.1007/s00769-024-01597-8 SN - 1432-0517 VL - 29 SP - 293 EP - 301 PB - Springer Science and Business Media LLC AN - OPUS4-59954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Hoppe, Marion A1 - Roik, Janina T1 - Certification of a soda–lime–silica glass reference material for XRF-analysis N2 - The preparation, analysis and certification of a new certified glass reference material (CRM) for multi-element determination in soda–lime–silica glass is described. The CRM BAM-S006 is available in the form of discs (thickness: 5 mm, diameter: 40 mm) as well as in form of cullet. Certified properties are the mass fractions of 19 main, minor and trace elements. The certified values are based on the results of 18 laboratories which participated in the certification inter-laboratory comparison. The CRM is intended for establishing or checking the calibration of x-ray spectrometers for the analysis of samples of similar matrix composition as well as for wet chemical analysis. KW - reference material KW - soda-lime-silica glass KW - XRF-analysis PY - 2025 DO - https://doi.org/10.13036/17533562.66.2.04 SN - 1753-3562 VL - 66 IS - 2 SP - 58 EP - 62 PB - Society of Glass Technology CY - Sheffield, UK AN - OPUS4-64543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blanchard, V. A1 - Traub, Heike T1 - Central project for biochemical analysis of proteoglycans and glycosaminoglycans and for element-specific microscopy N2 - Nearly all disease processes are associated with variations of components of the extracellular matrix (ECM) that are typically observed during the development of inflammation. This concerns for example proteoglycans and their associated glycosaminoglycans (GAG), which have been shown to bind to cationic metal imaging probes due to their strong complexing activity. The complexing activity largely depends on the degree of GAG sulfation and/or carboxylation as well as on the GAG isomericity. In this central project, we investigate GAG structures from inflammatory disorders (namely cardiovascular diseases, inflammatory intestinal diseases and neuroinflammation) provided by researchers of the Collaborative Research Center at the molecular disaccharidic level using chromatographic and mass spectrometric methods. In parallel, the spatial localization and quantification of metal-based imaging probes are evaluated by LA-ICP-MS imaging. T2 - 1st International Symposium In vivo Visualization of Extracellular Matrix Pathology CY - Online Meeting DA - 27.05.2021 KW - Laser ablation KW - ICP-MS KW - MALDI PY - 2021 AN - OPUS4-52716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kepsutlu, B. A1 - Wycisk, V. A1 - Achazi, K. A1 - Kapishnikov, S. A1 - Perez-Berna, A.J. A1 - Guttmann, P. A1 - Cossmer, Antje A1 - Pereiro, E. A1 - Ewers, H. A1 - Ballauff, M. A1 - Schneider, G. A1 - McNally, J.G. T1 - Cells Undergo Major Changes in the Quantity of Cytoplasmic Organelles after Uptake of Gold Nanoparticles with Biologically Relevant Surface Coatings N2 - Here, we use cryo soft X-ray tomography (cryo-SXT), which delivers 3D ultrastructural volumes of intact cells without chemical fixation or staining, to gain insight about nanoparticle uptake for nanomedicine. We initially used dendritic polyglycerol sulfate (dPGS) with potential diagnostic and therapeutic applications in inflammation. Although dPGS-coated gold nanoparticle (dPGS-AuNP) uptake followed a conventional endocytic/degradative pathway in human lung epithelial cell lines (A549), with cryo-SXT, we detected ∼5% of dPGS-AuNPs in the cytoplasm, a level undetectable by confocal light microscopy. We also observed ∼5% of dPGS-AuNPs in a rarely identified subcellular site, namely, lipid droplets, which are important for cellular energy metabolism. Finally, we also found substantial changes in the quantity of cytoplasmic organelles upon dPGS-AuNP uptake over the 1–6 h incubation period; the number of small vesicles and mitochondria significantly increased, and the number of multivesicular bodies and the number and volume of lipid droplets significantly decreased. Although nearly all organelle numbers at 6 h were still significantly different from controls, most appeared to be returning to normal levels. To test for generality, we also examined cells after uptake of gold nanoparticles coated with a different agent, polyethylenimine (PEI), used for nucleic acid delivery. PEI nanoparticles did not enter lipid droplets, but they induced similar, albeit less pronounced, changes in the quantity of cytoplasmic organelles. We confirmed these changes in organelle quantities for both nanoparticle coatings by confocal fluorescence microscopy. We suggest this cytoplasmic remodeling could reflect a more common cellular response to coated gold nanoparticle uptake. KW - Cellular trafficking KW - Confocal laser scanning microscopy KW - Cytoplasmic remodeling KW - Dendritic polyglycerol sulfate KW - Polyethylenimine KW - 3D ultrastructural analysis KW - Cryo-soft X-ray tomography PY - 2020 DO - https://doi.org/10.1021/acsnano.9b09264 VL - 14 IS - 2 SP - 2248 EP - 2264 AN - OPUS4-50464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oskoei, Párástu T1 - Cell mechanisms induced by doxorubicin-loaded UCNP@MSN nanoparticles with a thermosresponsive nanovalve in melanoma cells N2 - Upconversion nanoparticles (UCNPs) exhibit several remarkable optical properties, including excitation by near infrared (NIR) light, which enables deep tissue penetration, multiple distinct emission bands across a wide range of wavelengths, long luminescen ce lifetimes, and high photostability. These features make them particularly attractive for various biomedical applications. Mesoporous silica nanoparticles (MSNs), functionalized with nanovalves or specific coatings, have been explored for controlled and targeted drug delivery, where therapeutic agents are encapsulated within the nanopores, allowing spatiotemporal release 1 3 ]]. Among the promising approaches, photoactivated drug delivery systems have drawn considerable interest due to their versatility and potential. One relevant application is in the treatment of melanoma, an aggressive form of skin cancer with a rising global incidence. In advanced stages, conventional therapies often fail to achieve complete tumour eradication, resulting in poor prognose s 4 In this study, UCNPs were coated with a mesoporous silica shell to form core shell UCNP@MSN nanoparticles, which were further functionalized with thermoresponsive retro Diels Alder nanovalves and loaded with doxorubicin (DOX), a chemotherapeutic drug used in melanoma treatment. Upon exposure to 980 nm NIR light, DOX release was successfully triggered in the culture medium. Exposure to functionalized UCNPs decreased the viability of the tested melanoma cell lines, with further reductions observed when the ex posure to the nanoparticles was combined with irradiation. Subsequently, t he toxicity mechanisms were evaluated and showed that w hile individual treatments with either the functionalized UCNPs or NIR irradiation alone had no effect on reactive oxygen species (ROS) production, their combination significantly increased ROS levels in two of the three tested cell lines. This combined treatment also led to notable increases in apoptotic , necrotic or both type of cells’ percentages on all cell lines. Overall, these findings highlight the potential of these nanoparticles with thermoresponsive gating mechanisms as effective platforms for targeted drug delivery in melanoma therapy. T2 - EUROTOX 2025 CY - Athens, Greece DA - 14.09.2025 KW - Nano KW - Particle KW - Lanthanide KW - Upconversion KW - Surface chemistry KW - Mesoporous silica KW - Doxorubicin KW - Nanomedicine KW - Triggered release KW - pH KW - Cellular uptake KW - Toxicity KW - Folate KW - Ligand PY - 2025 AN - OPUS4-64372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM-P213: BAM procedure for obtaining Cu delta values N2 - BAM participated in the CCQM pilot study P213 for obtaining copper isotope delta values. This presentations provides details on the MC-ICP-MS based measruement procedure, which has been applied to obtain such copper delta values. T2 - IRWG Meeting CY - Online meeting DA - 12.05.2022 KW - Isotope delta value KW - Copper KW - Metrology KW - Traceability PY - 2022 AN - OPUS4-55162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM-P213: BAM procedure for obtaining Cu delta values N2 - BAM participated in the CCQM pilot study P213 for obtaining copper isotope delta values. This presentations provides details on the MC-ICP-MS based measruement procedure, which has been applied to obtain such copper delta values. T2 - IRWG Meeting 2022 CY - Online meeting DA - 20.09.2022 KW - Isotope ratio KW - Copper KW - Metrology KW - Traceability KW - Uncertainty PY - 2022 AN - OPUS4-55864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hill, Sarah A1 - Infante, Heidi Goenaga A1 - Entwisle, John A1 - Strekopytov, Stanislav A1 - Ward-Deitrich, Christian A1 - Cowen, Simon A1 - Rienitz, Olaf A1 - Roethke, Anita A1 - Goerlitz, Volker A1 - Schulz, Ursula A1 - Pape, Carola A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Jacimovic, Radojko A1 - Fisicaro, Paola A1 - Ren, Tongxiang A1 - Wang, Song A1 - Song, Panshu A1 - Li, Haifeng A1 - Linsky, Maré A1 - Sobina, Egor A1 - Lozano, Hernán Ezequiel A1 - Puelles, Mabel A1 - Yamani, Randa A1 - Haraldsson, Conny T1 - CCQM-K160: platinum group elements in automotive catalyst N2 - The platinum group elements (PGEs) play an important role in reducing emissions from automotive vehicles through their use in catalytic convertors but also for catalysis in the pharmaceutical industry. The immense economic value of platinum (Pt), palladium (Pd) and rhodium (Rh) highlights the importance of highly accurate measurements. Therefore, there is a need for National Metrology Institutes (NMIs) and Designated Institutes (DIs) to demonstrate measurement capability in this space. A pilot comparison (CCQM-P63) for precious metals in automotive catalyst took place in 2006, but with a limited number of institutes participating. Furthermore, this study was performed over 17 years ago. Therefore, there was a need to maintain existing capability and demonstrate new capability in a key comparison, in order to claim calibration and measurement capability claims (CMCs). With the core capability matrix, this study falls into the "Difficult to dissolve metals/metal oxides" which will support CMC categories 8 (Metal and metal alloys), 9 (Advanced materials) and 14 (Other materials). Eleven NMIs and DIs participated in the Key Comparison CCQM-K160 Platinum Group Elements in Automotive Catalyst. Participants were requested to evaluate the mass fractions of Pt, Pd and Rh in mg/kg in an unused autocatalyst material (cordierite ceramic base). The Key Comparison Reference Values (KCRVs) and Degrees of Equivalence (DoEs) were calculated utilising the NIST Decision Tree for the measurands. The participants utilised a number of sample preparation and analytical methods including hot plate digestion, microwave digestion and sodium fusion, followed by either atomic absorption spectroscopy (AAS), inductively coupled plasma optical emission spectroscopy (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS) detection. Several calibration techniques were used, namely external calibration, standard addition, isotope dilution mass spectrometry (IDMS) and an exact matching procedure. Additionally, one participant employed instrumental neutron activation analysis (INAA) with k0 standardisation which is a direct solid analysis method. The majority of participants claimed traceability to NIST primary calibrants or their own CRMs. Furthermore, several matrix CRMs were included or spiked samples for quality control. All institutes were required to determine the dry mass fraction using the stipulated protocol. The NIST decision tree was implemented for the calculation of the KCRVs and DoEs. The participant results overall showed good agreement with the KCRV, despite the variety of dissolution procedures and measurement techniques for this highly complex matrix and challenging measurands. Successful participation in CCQM-K160 demonstrated measurement capabilities for the determination of mass fraction of Pt, Pd and Rh in the mg/kg range and will support broad scope CMC claims for a wide range of challenging matrices. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - Metrology in Chemistry KW - Traceability KW - Uncertainty PY - 2024 DO - https://doi.org/10.1088/0026-1394/61/1A/08011 VL - 61 IS - 1A SP - 1 EP - 39 PB - IOP Publishing AN - OPUS4-60524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, X.M. A1 - Li, H.M. A1 - Zhang, Q.H. A1 - Lu, X.H. A1 - Li, S.Q. A1 - Koch, Matthias A1 - Polzer, J. A1 - Hackenber, R. A1 - Moniruzzaman, M. A1 - Khan, M. A1 - Kakoulides, E. A1 - Pak-Wing, K. A1 - Richy, A1 - Chi-Shing, N. A1 - Lu, T. A1 - Gui, E.M. A1 - Cheow, P.S. A1 - Teo, T.L. A1 - Rego, E. A1 - Garrido, B. A1 - Carvalho, L. A1 - Leal, R. A1 - Violante, F. A1 - Baek, S.Y. A1 - Lee, S. A1 - Choi, K. A1 - Kim, B. A1 - Bucar-Miklavcic, M. A1 - Hopley, C. A1 - Nammoonnoy, J. A1 - Murray, J. A1 - Wilson, W. A1 - Toman, B. A1 - Itoh, N. A1 - Gokcen, T. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K146 low-polarity analyte in high fat food: benzo a pyrene in olive oil N2 - The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix. KW - Metrology KW - CCQM KW - Food KW - PAH PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1a/08017 VL - 57 IS - 1a SP - 08017 AN - OPUS4-52435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Molloy, J. L. A1 - Winchester, M. R. A1 - Butler, T. A. A1 - Possolo, A. M. A1 - Rienitz, O. A1 - Roethke, A. A1 - Goerlitz, V. A1 - Caciano de Sena, R. A1 - Dominguez Almeida, M. A1 - Yang, L. A1 - Methven, B. A1 - Nadeau, K. A1 - Romero Arancibia, P. A1 - Bing, W. A1 - Tao, Z. A1 - Snell, J. A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Kotnala, R. K. A1 - Swarupa Tripathy, S. A1 - Elishian, C. A1 - Ketrin, R. A1 - Suzuki, T. A1 - Oduor Okumu, T. A1 - Yim, Y.-H. A1 - Heo, S. W. A1 - Min, H. S. A1 - Sub Han, M. A1 - Lim, Y. A1 - Velina Lara Manzano, J. A1 - Segoviano Regalado, F. A1 - Arvizu Torres, M. A1 - Valle Moya, E. A1 - Buzoianu, M. A1 - Sobina, A. A1 - Zyskin, V. A1 - Sobina, E. A1 - Migal, P. A1 - Linsky, M. A1 - Can, S. Z. A1 - Ari, B. A1 - Goenaga Infante, H. T1 - CCQM-K143 Comparison of Copper Calibration Solutions Prepared by NMIs/DIs N2 - CCQM-K143 is a key comparison that assesses participants’ ability to prepare single element calibration solutions. Preparing calibration solutions properly is the cornerstone of establishing a traceability link to the International System of Units (SI), and therefore should be tested in order to confirm the validity of CCQM comparisons of more complex materials. CCQM-K143 consisted of participants each preparing a single copper calibration solution at 10 g/kg copper mass fraction and shipping 10 bottled aliquots of that solution to the coordinating laboratory, the National Institute of Standards and Technology (NIST). The masses and mass fraction for the prepared solutions were documented with the submitted samples. The solutions prepared by all participants were measured at NIST by high performance inductively coupled plasma optical emission spectroscopy (HP-ICP-OES). The intensity measurements for copper were not mapped onto values of mass fraction via calibration. Instead, ratios were computed between the measurements for copper and simultaneous measurements for manganese, the internal standard, and all subsequent data reductions, including the computation of the KCRV and the degrees of equivalence, were based on these ratios. Other than for two participants whose measurement results appeared to suffer from calculation or preparation errors, all unilateral degrees of equivalence showed that the measured values did not differ significantly from the KCRV. These results were confirmed by a second set of ICP-OES measurements performed by the Physikalisch-Technische Bundesanstalt (PTB). CCQM-K143 showed that participants are capable of preparing calibration solutions starting from high purity, assayed copper metal. Similar steps are involved when preparing solutions for other elements, so it seems safe to infer that similar capabilities should prevail when preparing many different, single-element solutions. KW - Metrology KW - Primary calibration solution KW - Traceability PY - 2020 DO - https://doi.org/10.1088/0026-1394/58/1A/08006 SN - 0026-1394 VL - 58 IS - 1A SP - 08006 PB - IOP Science CY - Cambridge AN - OPUS4-51983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Jährling, R. A1 - Noordmann, J. A1 - Pape, C. A1 - Röhker, K. A1 - Vogl, Jochen A1 - Manzano, J. V. L. A1 - Kozlowski, W. A1 - Caciano de Siena, R. A1 - Marques Rodrigues, J. A1 - Galli, A. H. A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Lee, J. H. A1 - Min, H.-S. A1 - Chingbo, C. A1 - Naijie, S. A1 - Qian, W. A1 - Ren, T. A1 - Jun, W. A1 - Tangpaisarnkul, N. A1 - Suzuki, T. A1 - Nonose, N. A1 - Mester, Z. A1 - Yang, L. A1 - Pagliano, E. A1 - Greenberg, P. A1 - Mariassy, M. A1 - Näykki, T. A1 - Cankur, O. A1 - Coskun, F. G. A1 - Ari, B. A1 - Can, S. Z. T1 - CCQM-K122 "Anionic impurities and lead in salt solutions" N2 - The determination of the mass fractions of bromide, sulfate, and lead as well as the isotopic composition of the lead (expressed as the molar mass and the amount fractions of all four stable lead isotopes) in an aqueous solution of sodium chloride with a mass fraction of 0.15 g/g was the subject of this comparison. Even though the mass fractions ranged from 3 μg/g (bromide) to 50 ng/g (lead), almost all results reported agreed with the according KCRVs. KW - Absolute isotope ratio KW - Lead isotope ratios KW - Metrology KW - Traceability PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1A/08012 VL - 57 IS - 1A SP - 8012 PB - IOP Science AN - OPUS4-51156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, X.Q. A1 - Li, H.M. A1 - Jiao, H. A1 - Guo, Z.H. A1 - Zhang, Q.H. A1 - Kneeteman, L.E. A1 - Lewin, M. A1 - Pires do Rego, E.C. A1 - Leal, R.V. A1 - Violante, F.G.M. A1 - Riedel, Juliane A1 - Koch, Matthias T1 - CCQM Key Comparison track A CCQM-K168: Non-polar analytes in high carbohydrate food matrix: trans-zearalenone in maize powder N2 - Demonstrating competency and equivalence for the measurement capacity of contaminants and nutrients in primary foodstuffs is a priority of the OAWG 10-year strategy for Track A core comparisons. Such measurements have posed significant challenges for reference material producers and calibration service providers. This key comparison (KC), under the topic of “non- polar analyte in high carbohydrate food matrix: trans-Zearalenone (trans-ZEN) in maize powder” , was a sector of the model system selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to demonstrate the Calibration and Measurement Capabilities (CMCs) of national metrology institutes (NMIs) and designated institutes (DIs). 17 NMIs and DIs participated in the Track A KC CCQM- 168 “non-polar analyte in high carbohydrate food matrix: trans-ZEN in maize powder” . Participants were requested to evaluate the mass fraction (μg/kg) of trans-ZEN in maize powder material. Methods like liquid-liquid extraction and SPE were applied in the pre-treatment, and HPLC-MS/MS and HPLC-FLD were used for detection by the participants. The mass fractions for trans-ZEN were in the range of (91.8 to 169) μg/kg with standard uncertainties of (1.5 to 24.7) μg/kg, and corresponding relative standard uncertainties from 1.5% to 14.6%. Two labs, INTI and BAM were excluded from the KCRV evaluation. INTI result was identified as an outlier and confirmed their method had insufficient specificity. For BAM the calibration approach they used does not meet the CIPM traceability requirements. The other 15 labs included in the calculation of the consensus KCRV all agreed within their standard uncertainties. Hierarchical Bayes was used as estimators in calculating KCRV and standard uncertainty. Successful participation in CCQM-K168 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 1 μg/kg to 1000 μg/kg in a high carbohydrate food matrix. KW - Metrology KW - Quality Assurance KW - Mycotoxin Analysis KW - Sustainable Food Safety PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08021 VL - 60 IS - 1a SP - 08021 AN - OPUS4-59059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM IRWG draft strategy for all elements except for noble gases and H, C, N, O N2 - The presentation describes the draft strategy for metalloids and semi-metals within the IRWG at CCQM. This includes the definition of the measurements space, a suitable set of key comparisons and pilot studies and a proposal for a harmonized CMC application. T2 - EURAMET TC-MC Workshop on Isotope Ratio Analysis CY - Bern, Switzerland DA - 05.02.2020 KW - CMC KW - Measurement space KW - Metrology KW - Isotope ratio PY - 2020 AN - OPUS4-50345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fiedler, Saskia T1 - Cathodoluminescence Spectroscopy of Silicon Nanoparticles N2 - The fabrication of nanostructures with ever-decreasing sizes has increased the demand of suitable characterization methods which allow to determine their shape and size at the true nanoscale, and similarly important, enable the investigation of their optical properties beyond the diffraction limit. Due to its high spectral and spatial resolution down to the (sub-) nanometer range, electron beam-based techniques, namely cathodoluminescence (CL) has become a powerful characterization tool, particularly to study plasmonic and dielectric nanostructures. However, the interpretation of the resulting spectral CL maps is not always unambiguously straightforward. In this work, Mie resonances in single Si nanospheres of different sizes have been systematically studied, using experimental CL spectroscopy and an analytical CL model. For smaller spheres (r ~ 75 nm), the eigenmodes can be unequivocally identified, with relative changes in intensity of the electric and magnetic dipole depending on the electron beam position within the sphere. However, in larger spheres (r ~ 105 nm), the modal assignment becomes increasingly difficult due to a larger number of Mie modes in the visible spectral range. Additionally, penetrating electron beams generate two radiating dipoles at the two Si interfaces – due to the electron and its image charge collapsing at those interfaces – which can, depending on the electron beam’s velocity and its path length inside the particle, produce distinct resonances or dips (constructive or destructive interference of those two radiative dipoles). It is demonstrated that superimposed on the eigenmodes of the studied nanospheres, these resonances can distort the recorded spectrum and lead to potentially erroneous assignment of modal characters to the spectral features. An intuitive analogy is developed to unambiguously distinguish those resonance induced by transition radiation from the nanoparticle-specific Mie resonances. T2 - Optoelectronic Processes at Nanostructured Interfaces 2022 CY - Bad Honnef, Germany DA - 21.03.2022 KW - Cathodoluminescence KW - Silicon nanoparticles KW - Mie resonances PY - 2022 AN - OPUS4-54526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Career Options in Public Service N2 - In the following, an overview of possible career options for chemists is presented covering metrology institutes, departmental research institutes of ministries, Federal and state research institutes and options in areas such as Federal or state institutions in charge of occupational safety, the German armed forces, wastewater treatment plants and labs/institutes controlling water quality, and museums. Thereby also examples and personal insights of the daily work routine are provided for some employers. T2 - Career-Workshop ChiÖD CY - Karlsruhe, Germany DA - 02.04.2025 KW - Quality assurance KW - Reference analysis KW - Standardization KW - Metrology KW - Reference products KW - Reference materials KW - Mission PY - 2025 AN - OPUS4-62867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinelt, Manuel T1 - Capabilities of Surface-Assisted Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (SA-FAPA-MS) for Direct Analysis of Polycyclic Aromatic Hydrocarbons (PAHs) N2 - Ambient desorption/ionization mass spectrometry (ADI-MS) is a growing area in the analytical chemistry of organic molecules. It requires only minimal sample preparation and can reduce analysis time compared to traditional methods.[1] One evolving method is the plasma-based pin-to-capillary Flowing Atmospheric-Pressure Afterglow (FAPA) source. Which is an improved version of the original pin-to-plate FAPA, resulting in significantly lower background signals and less oxidation of the analytes.[2] In our case, samples are probed directly from thin-layer chromatography (TLC) plates, which have shown promising results in improving signal response and performance in mass spectral imaging in previous studies. Especially, cyano (CN)-HPTLC and reversed-phase (RP2)-TLC plates were suited best for the analysis of different organic molecules.[3] In this work, FAPA is investigated as a method to determine polycyclic aromatic hydrocarbons (PAHs). Furthermore, its suitability for rapid screening of real samples was investigated. 30 pure PAH standard samples were analyzed on different TLC surfaces. Cyano (CN)-HPTLC and reversed-phase (RP2)-TLC plates proved to be the most suitable substrate for the analysis of PAH compounds. Linear ranges of up to four orders of magnitude could be achieved. Limits of detection (LOD) of anthracene, chrysene, and fluorene were in the µg/L range. However, these pure analytes differ from PAH samples collected in the environment, which may contain hundreds of different PAHs among other constituents. Therefore, PAH containing real samples were used to test the method and its screening capability on more complex samples. A standard reference material (diesel particulate extract, NIST SRM 1975) was analyzed for method validation. For sample preparation, 1 µL of the extract was spotted directly onto the TLC surface. It was possible to perform a triple determination in approx. 20 min. Therefore, SA-FAPA-MS has a huge potential to be established as a method for rapid qualitative screening of PAHs in real samples. T2 - 55th Annual Conference of the German Society for Mass Spectrometry (Deutsche Gesellschaft für Massenspektrometrie, DGMS). CY - Freising, Germany DA - 10.03.2024 KW - Mass Spectrometry KW - Massenspektrometrie KW - Instrumental Analytical Chemistry KW - Instrumentelle Analytische Chemie KW - Polycyclic Aromatic Hydrocarbons PY - 2024 AN - OPUS4-62316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munir, R. A1 - Noureen, N. A1 - Bashir, M. A1 - Shoaib, N. A1 - Ashraf, A. A1 - Lisec, Jan A1 - Zaidi, N. T1 - Cancer Awareness Measure (CAM) and Cancer Awareness Measure MYthical Causes Scale (CAM‑MY) scores in Pakistani population N2 - Lifestyle modifications could prevent almost one‑third to one‑half of all cancer cases. The awareness of cancer risk factors could motivate people to make such changes in their behaviors and lifestyles. This work aims to investigate the cancer awareness level in the Pakistani population. Telephone interviews of 657 individuals in Pakistan were carried out using the Cancer Awareness Measure (CAM) and Cancer Awareness Measure–MYthical Causes Scale (CAM‑MY). We observed that participants scored significantly better on the CAM scale than the CAM‑MY scale, and CAM scores were negatively associated with CAM‑MY scores. Years of formal education or a biology major at undergraduate or graduate level did not affect our population’s cancer awareness levels. Age displayed a weak but statistically significant negative association with CAM scores. Most participants failed to identify modifiable cancer risk factors, e.g., low physical activity. Efforts should be made to improve awareness of modifiable risk factors. We observed that brief training sessions could markedly improve people’s understanding of cancer risk factors and myths. KW - Cancer KW - Cancer awareness measure KW - Cancer risk PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548960 DO - https://doi.org/10.1038/s41598-022-13012-8 SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 10 PB - Nature Publishing Group CY - London AN - OPUS4-54896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Gornushkin, Igor B. ED - Galbács, G. T1 - Calibration-Free Quantitative Analysis N2 - Calibration-free methods in laser-induced breakdown spectroscopy, CF LIBS, serve as an alternative to calibration-based LIBS techniques. Their major advantage is the ability for fast chemical analysis in situations where matrix-matched standards are not readily available (as, e.g., in the analysis of biological materials and remote analysis) or amount of samples are limited. Their main applications are in the industry, geology, biology, archeology, and even space exploration. This chapter overviews the principle of operation and performance of CF LIBS techniques. KW - Laser induced plasma KW - Calibration-free LIBS PY - 2022 SN - 978-3-031-14501-8 DO - https://doi.org/10.1007/978-3-031-14502-5 SP - 67 EP - 100 PB - Springer Nature Switzerland AG AN - OPUS4-56651 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bornemann-Pfeiffer, Martin A1 - Kern, Simon A1 - Maiwald, Michael A1 - Meyer, Klas T1 - Calibration-Free Chemical Process and Quality Control Units as Enablers for Modular Production N2 - Modular chemical production is a tangible translation of the digital transformation of the process industry for specialty chemicals. In particular, it enables the speeding-up of process development and thus a quicker time to market by flexibly connecting and orchestrating standardised physical modules and bringing them to life (i.e., parameterising them) with digitally accumulated process knowledge. We focus on the specific challenges of chemical process and quality control, which in its current form is not well suited for modular production and provide possible approaches and examples of the change towards direct analytical methods, analytical model transfer or machine-supported processes. KW - Modular Production KW - Chemical Process Control KW - Process Analytical Technology KW - Digital Transformation KW - Industry 4.0 PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517264 DO - https://doi.org/10.1002/cite.202000150 SN - 1522-2640 VL - 93 IS - 1-2 SP - 62 EP - 70 PB - Wiley-VCH CY - Weinheim AN - OPUS4-51726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Calibration of Mg isotope amount ratios and delta values N2 - In the past, δ26/24Mg measurements were referenced to NIST SRM 980, the initial zero of the δ26/24Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. To solve this problem a suite of magnesium isotope reference materials, ERM-AE143, -AE144 and -AE145, has been certified in a first study by applying an ab initio calibration for absolute Mg isotope ratios without any a priori assumptions, a procedure which fulfils all requirements of a primary method of measurement. We could achieve for the first time measurement uncertainties for isotope amount ratios close to the typical precision of magnesium delta values, δ26/24Mg, which are at the 0.1 ‰ level (2SD). In addition, it was demonstrated that commonly used fractionation laws are invalid for correcting Mg isotope ratios in multi-collector ICPMS as they result in a bias which is not covered by its associated uncertainty. Depending on their type, fractionation laws create a bias up to several per mil, with the exponential law showing the smallest bias between 0.1 ‰ to 0.7 ‰. With these isotope reference materials, it is possible to establish SI-traceability for magnesium delta measurements. To realize this, we organized a second study within which five expert laboratories participated to cross-calibrate all available magnesium isotope standards, which are NIST SRM 980, IRMM-009, ERM-AE143, ERM-AE144, ERM-AE145 and the standards DSM3 and Cambridge-1. The mean δ26/24Mg values for the individual iRMs, calculated from the laboratory means show 2 SD reproducibilities varying between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for δ26/24Mg determinations (2SD). Thus, SI traceability for magnesium isotope amount ratios and delta values is demonstrated to be established. T2 - 53rd annual conference of the DGMS including 27th ICP-MS User's Meeting CY - Münster, Germany DA - 01.03.2020 KW - Isotope ratio KW - Delta value KW - Metrology KW - Magnesium KW - Magnesium isotope ratios PY - 2020 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-50549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, V. A1 - Uhlemann, M. A1 - Richter, Silke A1 - Pfeifer, jens T1 - Calibration capacity of hot-pressed hydrogen standards for glow discharge optical emission and mass spectrometry N2 - Mixed copper and titanium hydride powder was hot-pressed and characterized by Carrier Gas Hot Extraction, XRay Diffraction, Thermal Gravimetric Analysis coupled with Mass Spectrometry, and Scanning Electron Microscopy. The hot-pressed and five conventional samples were applied for calibration of hydrogen in Glow Discharge Optical Emission and Mass Spectrometry. Up to the introduction of 15 ng/s hydrogen the Emission yield model is useful in Glow Discharge Optical Emission Spectrometry. A correlation between saturation and even reversal of the emission yield of the spectral lines H121, H486 and H656 and low sputtering rates was found. Hydrogen effects exist for the spectral lines of Cu(II) 219 and Ti(I) 399. In Glow Discharge Mass Spectrometry, a linear dependency of the 1H ion current on the sputtered mass per time exists over the total range of hydrogen content investigated. Hydrogen effects also exist for the sensitivity of 48Ti and 63Cu. The sputtering rate of two-phase materials depends linearly on the sputtered mass per time of one phase, which allows the sputtering rate of two-phase materials with known composition to be predicted. KW - Hot-pressing KW - GD-OES KW - GD-MS KW - Calibration KW - Hydrogen KW - Titanium hydride KW - Sputtering KW - Two-phase system PY - 2021 DO - https://doi.org/10.1016/j.sab.2020.106039 VL - 176 SP - 106039 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-52074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stein, L. A1 - Wang, Cui A1 - Förster, C. A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Bulky ligands protect molecular ruby from oxygen quenching N2 - Chromium(III) complexes can show phosphorescence from the spin-flip excited doublet states 2E/2T1 in the near-infrared with high photoluminescence quantum yields and extremely long lifetimes in the absence of dioxygen. The prototype molecular ruby, [Cr(ddpd)2]3+ (ddpd = N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine), has a photoluminescence quantum yield and a luminescence lifetime of 13.7% and 1.1 ms in deaerated acetonitrile, respectively. However, its luminescence is strongly quenched by 3O2 via an efficient Dexter-type energy transfer process. To enable luminescence applications of molecular rubies in solution under aerobic conditions, we explored the potential of sterically demanding ddpd ligands to shield the chromium(III) center from O2 using steady state and time-resolved photoluminescence spectroscopy. The structures of the novel complexes with sterically demanding ligands were investigated by single crystal X-ray diffraction and quantum chemically by density functional theory calculations. The O2 sensitivity of the photoluminescence was derived from absolutely measured photoluminescence quantum yields and excited state lifetimes under inert and aerobic conditions and by Stern–Volmer analyses of these data. Optimal sterically shielded chromium(III) complexes revealed photoluminescence quantum yields of up to 5.1% and excited state lifetimes of 518 μs in air-saturated acetonitrile, underlining the large potential of this ligand design approach to broaden the applicability of highly emissive chromium(III) complexes. KW - Fluorescence KW - Synthesis KW - Production KW - Optical spectroscopy KW - Ligand KW - Photophysics KW - Cr(III) KW - Mechanism KW - NIR KW - Sensor KW - Oxygen PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570807 DO - https://doi.org/10.1039/d2dt02950b VL - 51 IS - 46 SP - 17664 EP - 17670 PB - The Royal Society of Chemistry CY - Berlin AN - OPUS4-57080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - Breaking the Wall of Environmental Pollutants N2 - With the continuous release of anthropogenic pollutants into the environment, substantial risks for the human health arise. Concerning are especially persistent substances (e.g., PFAS) as they accumulate in food chains which inevitably result in the transgression of negative impact threshold levels. Environmental Analytical Chemsitry interfaces all disciplines of Risk Assessment. Therefore it is the important tool to identify, monitor, and remediate environmental pollutants. Based on the example of PFAS, a workflow to tackle environmental pollutants in a retro- and pro-spective way is shown. Within the project, the worldwide situation of environmental pollutants will be illustrated for the example of PFAS. As the major discipline to confront the problem, analytical chemistry will be shown as a key tool for contesting PFAS and creating safe-by-design materials in the future. T2 - Falling Walls Lab 2023 CY - Berlin, Germany DA - 21.09.2023 KW - PFAS KW - Analytical Chemistry KW - Environmental pollutants KW - Risk assessment PY - 2023 AN - OPUS4-58406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Temgoua, Ranil C. T. A1 - Lisec, Jan A1 - Koch, Matthias T1 - Breaking down phenylurea herbicides: advanced electrochemical approaches for environmental degradation and remediation N2 - Phenylurea herbicides (PUHs) represent one of the most extensively used herbicide families in agriculture worldwide. While effective for weed control, their environmental persistence, bioaccumulation potential, and formation of toxic metabolites raise significant environmental concerns. This review examines current electrochemical strategies for degrading phenylurea herbicides, with special emphasis on electrochemical oxidation (EC), photoelectrochemical processes (PEC), electro-Fenton (ECF) and photo-electro-Fenton (PECF), with particular attention to the various reactor configurations and their operational mechanisms. A critical innovation of this review lies in its systematic parameter assessment framework, which categorizes nine key operational parameters across all electrochemical degradation methods: electrode material, catalyst type, cell configuration, radiation source, operating conditions (pH, current density, temperature), removal efficiency, mineralization rate, degradation kinetics, identified intermediates, and Energy consumption. For each technique, we highlight which parameters are essential, important, critical, or non� applicable, providing a structured framework to guide future experimental design. Selected case studies are presented to illustrate practical applications and performance outcomes. The review concludes with acritical analysis of current knowledge gaps and future research avenues that could enhance the sustainability, efficiency, and scalability of electrochemical remediation technologies. This work is intended as a comprehensive resource for environmental chemists, analytical scientists, and remediation engineers committed to addressing phenylurea herbicide contamination. KW - Mass Spectrometry KW - Phenylurea herbicides KW - Electrochemistry PY - 2026 DO - https://doi.org/10.1039/D5EW00809C SN - 2053-1400 VL - 12 IS - 1 SP - 72 EP - 92 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xiao, J. A1 - Vogl, Jochen A1 - Rosner, M. A1 - Jin, Z. T1 - Boron isotope fractionation in soil-plant systems and its influence on biogeochemical cycling N2 - Boron (B) is an essential mineral nutrient for higher plants. Although B plant nutrition is well studied, the B isotope fractionation at the soil-plant interface, within plant metabolism, and its influence on biogeochemical cycling is not fully understood. Boron concentrations and isotope variations (δ11B) of the dicotyledonous plants of Chenopodium album and Brassica napus and their growing soils along a climatic gradient were analyzed to decipher these unresolved issues of the B behavior. The boron concentrations and δ11B values show an increasing trend from roots to leaves for both plants, while a decreasing trend from flower to shell and to seed for Brassica napus. A large boron isotope fractionation occurs within the plants with median Δ11Bleaf-root ≈ +20‰, which is related to different boron transporters and transportation ways. Formation of borate dimerized rhamnogalacturonan II in cell and B(OH)3 transportation in xylem lead to heavier δ11B values from root to stem and leaf while B(OH)4􀀀 transportation in phloem lead to lighter δ11B values from flower to shell and seed. Although samples cover a distinct transect with systematically different climatic conditions, Δδ11B within the individual plant compartments and between the bulk plants and the soil available B do not show any systematic variation. This suggests that B uptake from the soil into Chenopodium album and Brassica napus occurs without a distinct isotope fractionation at the soil-plant interface (median Δ11Bbulkplant-soil = 􀀀 0.2‰) and plants are able to regulate boron uptake. Both the observed large B fractionation within plant and low or absent B isotope fractionation at the soil-plant interface may have profound implications for the biological and geological B cycle. If this observed boron behavior also exists in other plants, their litters would be an important source for exporting 11B-rich biological material from continental ecosystems via rivers to the global oceans. This may be helpful for the explanation of ocean B cycle and the increasing δ11B values over the Cenozoic. KW - Boron isotopic composition KW - Boron isotope fractionation KW - Soil available boron KW - Biological boron recycling KW - Chenopodium album KW - Brassica napus PY - 2022 DO - https://doi.org/10.1016/j.chemgeo.2022.120972 SN - 0009-2541 VL - 606 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-55031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steglich, P. A1 - Mai, C. A1 - Bondarenko, S. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Schrader, S. A1 - Mai, A. T1 - BioPIC - Integration of Biosensors based on Photonic Integrated Circuits by Local-Backside Etching N2 - Silicon photonic sensors are promising candidates for lab-on-a-chip solutions with versatile applications and scalable production prospects using complementary metal-oxide semiconductor (CMOS) fabrication methods. However, the widespread use has been hindered because the sensing area adjoins optical and electrical components making packaging and sensor handling challenging. In this work, a local back-side release of the photonic sensor is employed, enabling a separation of the sensing area from the rest of the chip. This approach allows preserving the compatibility of photonic integrated circuits in the front-end of line and metal interconnects in the back-end of line. T2 - ATTRACT online Conference CY - Online meeting DA - 22.09.2020 KW - Silicon Photonics KW - Photonic Sensor KW - Photonic Integrated Circuits KW - Point-Of-Care-Diagnostics KW - CMOS KW - Microfluidics KW - Lab-on-a-chip KW - Ring resonator PY - 2020 UR - https://attract-eu.com/showroom/project/integration-of-biosensors-based-on-photonic-integrated-circuits-by-local-backside-etching-biopic/ SP - 1 EP - 5 AN - OPUS4-51735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind entscheidend für die Qualitätssicherung von Laboratorien. Diese nutzen Referenzmaterialien unter anderem zur Validierung von Messverfahren und zur Kalibrierung von Geräten. Dabei ist zu beachten, dass zertifizierte Merkmalswerte stets eine gewisse Unsicherheit aufweisen. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Artikels. Des Weiteren wird ein Vorgehen beschrieben, wie die Unsicherheit von Messverfahren mit Hilfe eines Referenzmaterials bestimmt werden kann. KW - Referenzmaterial KW - Messunsicherheit KW - Qualitätskontrolle PY - 2024 DO - https://doi.org/10.1515/teme-2024-0025 SN - 0171-8096 SP - 1 EP - 7 PB - De Gruyter AN - OPUS4-60564 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 - Meyer, Klas T1 - Benchtop NMR spectroscopy in chemical manufacturing: From hardware field integration to data modeling N2 - The use of benchtop-NMR instruments is constantly increasing during the recent years. Advantages of being affordable, portable and easy-to-operate without the need for trained staff make them especially interesting for industrial applications in quality control. However, applications of NMR spectroscopy as an online PAT tool are still very rare but offer a huge potential for process optimization and control. A key task to exploit this potential is hardware field integration of the lab-instruments in a rough environment of a chemical plant. Additionally, developments in automation and data evaluation are mandatory to ensure a robust unattended operation with low maintenance requirements. Here, we show an approach of a fully automated analyzer enclosure considering explosion safety, field communication, as well as environmental conditions in the field. Temperature sensitivity is still a limitation of benchtop-NMR instruments in flow applications. Recent developments of manufacturers allow for limited operation at static temperature levels, however, a dynamic system for continuous operation is still not available. Using a prototype system offering a larger bore, active temperature shielding studies with thermostated air were performed evaluating the performance. Automated data evaluation of NMR spectra using a modular indirect hard modeling (IHM) approach showed good results and flexibility. A second data analysis approach based on artificial neural networks (ANN) was evaluated.Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously, offering new ways to simultaneously evaluating large numbers of different models. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 24.05.2023 KW - Field integration KW - Benchtop-NMR KW - Process Analytical Technology PY - 2023 AN - OPUS4-57560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Resch-Genger, Ute A1 - Abram, Sarah-Luise A1 - Tavernaro, Isabella A1 - Zou, Shan A1 - Johnston, Linda T1 - Behind the Paper: Nanoscale Reference and Test Materials for the Validation of Characterization Methods for Engineered Nanomaterials – Current State, Limitations and Needs N2 - Engineered nanomaterials (NMs) of different material composition, morphology, and surface chemistry are widely used in material and life sciences. For NM quality control and risk assessment, NM key properties must be characterized with validated methods, requiring reference materials (RMs). KW - Engineered Nanomaterials KW - Nanoscale reference materials KW - Interlaboratory comparisons KW - Traceability KW - Standardization and Regulation KW - Nano KW - Particle KW - Quality assurance KW - Surface chemistry PY - 2025 UR - https://communities.springernature.com/posts/nanoscale-reference-and-test-materials-for-the-validation-of-characterization-methods-for-engineered-nanomaterials-current-state-limitations-and-needs SP - 1 EP - 3 PB - Springer Nature CY - Online AN - OPUS4-62572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -