TY - JOUR A1 - El-Athman, Rukeia A1 - Bresch, Harald A1 - Muth, Thilo A1 - Rädler, Jörg A1 - Rühle, Bastian T1 - Datenmanagement im Nanomaterial-Labor: Einsatz von ELN-Software zur digitalen Transformation des Laboralltags N2 - Angesichts der zunehmenden Digitalisierung und dem Einsatz datenintensiver Methodiken in der Wissenschaft stehen Forschende vor der Herausforderung, stetig wachsende Datenmengen nachvollziehbar zu dokumentieren, langfristig zu speichern und für Dritte nachnutzbar zu machen. Um diesen Anforderungen gerecht zu werden, bietet sich die Nutzung von Software-Lösungen an, welche Forschungsdatenmanagement mit der digitalen Dokumentation von Laborinventar und Experimenten in elektronischen Laborbüchern (engl. electronic lab notebooks (ELN)) verknüpfen. KW - NanoPlattform KW - BAM Data Store KW - OpenBIS KW - Forschungsdatenmanagement KW - Research data management KW - Elektronisches Laborbuch KW - Electronic lab notebook (ELN) PY - 2023 UR - https://analyticalscience.wiley.com/content/article-do/datenmanagement-im-nanomaterial-labor SN - 0016-3538 IS - 9 SP - 24 EP - 26 PB - Wiley Analytical Science CY - Weinheim AN - OPUS4-59600 LA - deu 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 - JOUR A1 - Gauglitz, Günter A1 - Bodensteiner, Michael A1 - Bohleber, Pascal A1 - Clases, David A1 - Dahms, Marcel A1 - Engelhard, Carsten A1 - Haider, Markus A1 - Hayen, Heiko A1 - Herbst‐Irmer, Regine A1 - Jäger, Martin A1 - Kramell, Annemarie E. A1 - Legner, Robin A1 - Matysik, Frank‐Michael A1 - Pöthig, Alexander A1 - Rädle, Matthias A1 - Seifert, Stephan A1 - Steinhauser, Georg A1 - Wolter, Kathrin T1 - Trendbericht Analytische Chemie 2024 N2 - Mehrdimensionale Trenntechniken sowie Kopplungstechniken verbessern weiter die Auflösung in der Analytik. In der Elementanalytik beeindrucken neue Entwicklungen der Massenspektrometrie mit induktiv gekoppeltem Plasma, in der Archäometrie zerstörungsfreie In‐situ‐Analysen. Der 3‐D‐Druck treibt die elektroanalytische Forschung voran, und die Prozessanalytik setzt auf Lab‐on‐a‐Chip und vermeldet Neues bei der Raman‐Spektroskopie mit Flüssigkernlichtleitern. KW - Analytische Chemie KW - Trenntechniken KW - Elementanalytik KW - Massenspektrometrie KW - Prozessanalytik PY - 2024 DO - https://doi.org/10.1002/nadc.20244139242 SN - 1868-0054 VL - 72 IS - 4 SP - 52 EP - 64 PB - Wiley CY - Weinheim AN - OPUS4-62155 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data Acquisition System for Single Particle Inductively Coupled Plasma Mass Spectrometry (spICP-MS) with Nanosecond Time Resolution N2 - This study presents our data acquisition system prototype for spICP-MS with nanosecond time resolution (nanoDAQ) and a matching data processing approach for nanosecond resolved single particle spICP-MS data. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables the detection of gold nanoparticles (AuNP) as small as 7.5 nm[1] with a commercial single quadrupole ICP-MS instrument. The acquired transient data is processed based on the temporal distance between detector events and the event density. It was shown that the inverse logarithm of the distance between detector events is proportional to the particle size and that the number of detector events corresponding to a particle signal distribution can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion.[1] The high data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leads to the main time limitation for analyses being merely the sample uptake time and rinsing step between analyte solutions. T2 - 55th Annual Conference of the German Society for Mass Spectrometry CY - Freising, Germany DA - 10.03.2024 KW - Nanoparticles KW - Mass Spectrometry KW - Instrumentation KW - spICP-MS PY - 2024 AN - OPUS4-62315 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 - Schardt, Annika A1 - Schmitt, Johannes A1 - Engelhard, Carsten T1 - Single particle inductively coupled plasma mass spectrometry with nanosecond time resolution N2 - In this proof-of-principle study, we present our contribution to single particle inductively coupled plasma mass spectrometry (spICP-MS) developments with a novel in-house built data acquisition system with nanosecond time resolution (nanoDAQ) and a matching data processing approach. The new system can continuously sample the secondary electron multiplier (SEM) detector signal and enables the detection of gold nanoparticles (AuNP) as small as 7.5 nm with the commercial single quadrupole ICP-MS instrument used in this study. Recording of the SEM signal by the nanoDAQ is performed with a dwell time of approximately 4 ns. A tailored method was developed to process this type of transient data, which is based on determining the temporal distance between detector events that is denoted as event gap (EG). We found that the inverse logarithm of EG is proportional to the particle size and that the number of detector events corresponding to a particle signal distribution can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. Due to the high data acquisition frequency, a statistically significant number of data points can be obtained in 60 s or less and the main time limitation for analyses is merely the sample uptake time and rinsing step between analyte solutions. At this stage, the data processing method provides average information on complete data sets only and will be adapted to enable particle-by-particle analysis with future hardware/software revision. KW - ICP-MS KW - Nanoparticles KW - Nanosecond time resolution KW - Single particle detection PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612706 DO - https://doi.org/10.1039/d3ja00373f SN - 1364-5544 SN - 0267-9477 VL - 39 IS - 2 SP - 389 EP - 400 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-61270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schardt, Annika A1 - Schmitt, Johannes A1 - Engelhard, Carsten T1 - Cover image for the article "Single particle inductively coupled plasma mass spectrometry with nanosecond time resolution" N2 - Image for the front cover of the issue 39(2) of the JAAS (Journal of Analytical Atomic Spectrometry). See Annika Schardt et al., pp. 389–400. Image reproduced by permission of Annika Schardt, Johannes Schmitt and Carsten Engelhard. KW - Analytical chemistry KW - Nanoparticles KW - Single-particle characterization KW - Instrumentation KW - spICP-MS PY - 2024 DO - https://doi.org/10.1039/D4JA90005G SN - 1364-5544 SN - 0267-9477 VL - 39 IS - 2 SP - 295 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-62156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shahsanaei, Majid A1 - Farahbakhsh, Nastaran A1 - Pour-Ali, Sadegh A1 - Schardt, Annika A1 - Orangpour, Setareh A1 - Engelhard, Carsten A1 - Mohajernia, Shiva A1 - Killian, Manuela S. A1 - Hejazi, Sina T1 - Synergistic enhancement of photocatalytic hydrogen production in TiO2 nanosheets through light-induced defect formation and Pt single atoms N2 - In this investigation, we present a direct method employing UV-light radiation to induce point defects, specifically Ti3+ and VO, onto the surface of TiO2 nanosheets (TiO2-NSs) and efficiently decorate them with Pt particles. The addition of the Pt precursor is carried out during rest periods following UV-light cessation (light-induced samples, LI) and during UV-light exposure (photo-deposited samples, PD). The size and distribution of Pt particles on both LI and PD TiO2-NSs are systematically correlated with varying resting times, enabling precise control over Pt loading. The characterization of various TiO2-NSs is extensively conducted using microscopy techniques (FESEM, TEM, and HAADF-STEM) and spectroscopy (XPS). Gas chromatography is also employed for the evaluation of the H2 photocatalytic performance of various samples. Our findings reveal that Pt particles deposit on the TiO2-NSs surfaces as nanoparticles under illumination. After a 5 minutes resting time, a combination of Pt single atoms (SAs) and clusters, with a maximum loading of 0.37 at%, is formed. Extending the resting time to 60 minutes results in a gradual reduction in Pt SAs and clusters, leading to the deposition of Pt nanoparticles with lower loadings. Notably, Pt SAs and clusters exhibit superior performance in hydrogen evolution, showcasing a remarkable 4000-fold increase over pristine TiO2-NSs. Additionally, sustained UV radiation during Pt addition in the photo-deposited samples results in the formation of Pt nanoparticles with lower loading compared to LI samples, consequently diminishing photocatalytic hydrogen production. This study not only provides insights into the controlled manipulation of Pt SAs on TiO2-NSs but also highlights their exceptional efficacy in hydrogen evolution, offering valuable contributions to the design of efficient photocatalytic systems for sustainable hydrogen generation. KW - Chemistry KW - Nanosheets KW - Hydrogen PY - 2024 DO - https://doi.org/10.1039/D4TA01809E VL - 12 IS - 29 SP - 18554 EP - 18562 PB - Royal Society of Chemistry (RSC) AN - OPUS4-61271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duarte Bernardino, Carolina A1 - Lee, Mihyun A1 - Ren, Qun A1 - Ruehle, Bastian T1 - Facile Spray-Coating of Antimicrobial Silica Nanoparticles for High-Touch Surface Protection N2 - The rising threat from infectious pathogens poses an ever-growing challenge. Metal-based nanomaterials have gained a great deal of attention as active components in antimicrobial coatings. Here, we report on the development of readily deployable, sprayable antimicrobial surface coatings for high-touch stainless steel surfaces that are ubiquitous in many healthcare facilities to combat the spread of pathogens. We synthesized mesoporous silica nanoparticles (MSNs) with different surface functional groups, namely, amine (MSN-NH2), carboxy (MSN-COOH), and thiol groups (MSN-SH). These were chosen specifically due to their high affinity to copper and silver ions, which were used as antimicrobial payloads and could be incorporated into the mesoporous structure through favorable host−guest interactions, allowing us to find the most favorable combinations to achieve antimicrobial efficacy against various microbes on dry or semidry high-touch surfaces. The antimicrobial MSNs were firmly immobilized on stainless steel through a simple two-step spray-coating process. First, the stainless steel surfaces are primed with sprayable polyelectrolyte solutions acting as adhesion layers, and then, the loaded nanoparticle dispersions are spray-coated on top. The employed polyelectrolytes were selected and functionalized specifically to adhere well to stainless steel substrates while at the same time being complementary to the MSN surface groups to enhance the adhesion, wettability, homogeneity, and stability of the coatings. The antimicrobial properties of the nanoparticle suspension and the coatings were tested against three commonly found pathogenic bacteria, Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli, as well as a fungal pathogen, Candida albicans. Especially MSN-SH loaded with silver ions showed excellent antimicrobial efficacy against all tested pathogens under application-relevant, (semi)dry conditions. The findings obtained here facilitate our understanding of the correlation between the surface properties, payloads, and antimicrobial activity and show a new pathway toward simple and easily deployable solutions to combat the spread of pathogens with the help of sprayable antimicrobial surface coatings. KW - Mesoporous silica nanoparticles KW - Thin films KW - Antimicrobial coatings KW - Spray-coating KW - Infectious diseases KW - Pathogen transmission KW - High-touch surfaces PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626269 DO - https://doi.org/10.1021/acsami.4c18916 SN - 1944-8252 SP - 1 EP - 13 PB - ACS Publications CY - Washington, DC AN - OPUS4-62626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kozdras, Mark T1 - Towards a Self-driving Lab for Nanoparticle Research N2 - Society is currently confronted with two global challenges, climate change and sustainable development. This reality reverberates amongst the leading nations of the world and is articulated as a priority by the United Nations through the Framework Convention on Climate Change and its seventeen Sustainable Development Goals. In 2016, under the Paris Accord, Mission Innovation, MI, emerged as a global response to climate change and developed eight innovation challenges to mitigate its effect, including Clean Energy Materials, IC6. This innovation challenge focused its efforts on accelerating the development and deployment of clean energy materials by more than a factor of ten through Materials Acceleration Platforms, MAPs – autonomous, self-driving materials laboratories and renewed itself under the current mandate as Materials for Energy, M4E. Self-driving labs deploy artificial intelligence, robotic automation and high-performance simulation and modeling in a closed loop system of material synthesis and characterization. An international ecosystem for accelerated materials discovery has been established and finds applications in many enabling materials technologies, including nanomaterials. The importance of nanomaterials to catalysis for hydrogen production and carbon dioxide conversion as well as energy storage in batteries is well known. In this work, the international efforts under Materials for Energy will be elaborated including the development of MINERVA - MAP for Intelligent Nanomaterial synthesis Enabled by Robotics for Versatile Applications. MINERVA was specifically built to include the specialized equipment required for the synthesis, characterization and closed-loop optimization of various nano- and advanced materials, ranging from simple inorganic (silica, metal, metal oxide) or polymeric nanoparticles to more complex core-shell architectures and materials with well-defined porosity or surface chemistry. Currently, we are investigating materials for applications in antimicrobial and antibiofouling surface coatings, sensor materials, as well as the reproducible synthesis of reference materials with this platform. T2 - Nanotek 2024 CY - Barcelona, Spain DA - 25.03.2024 KW - Self-driving Labs KW - SDLs KW - Advanced Materials KW - Autonomous Materials Discovery KW - Nanoparticles Synthesis and Characterization PY - 2024 AN - OPUS4-60382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald T1 - Anwendungen von maschinellem Lernen und KI an der BAM N2 - Im Austausch mit den anderen Bundesoberbehörden wurden die KI-Ansätze der verschiedenen Bundesoberbehörden zu spezifischen Themen der Nanowissenschaften präsentiert. Der Vortrag der BAM fokusiert sich auf die Themen "Self driving lab", semantische Segmentierung und Auswertung von elektronenmikroskopischen Bildern sowie die Generierung von ausführbaren Machineninstruktionen aus natürlicher Sprache. Abschließend wird der neue BAM DataStore vorgestellt. T2 - Nano-Behördenklausur 2024 CY - Berlin, Germany DA - 03.07.02024 KW - Nano KW - Bundesoberbehörden KW - Künstliche Intelligenz KW - Neuronale Netzwerke KW - Elektronisches Laborbuch PY - 2024 AN - OPUS4-61819 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Duarte Bernardino, Carolina T1 - Metal-Ion Loaded Silica Nanoparticles as Antimicrobial Coatings for Safer High-Touch Surfaces N2 - Not only since the Covid-19 pandemic have researchers focused their efforts on high touch surfaces to minimize the contraction of infectious diseases due to human contact. To help prevent the spread of infectious pathogens, surfaces and coatings are designed to minimize the presence or survivability of pathogens on surfaces in various settings, including healthcare centers, long-term care facilities, public transport, schools, and businesses. Extensive research has focused on finding solutions to prevent bacterial transmission and biofilm formation by killing or reducing the attachment of microbes. These solutions include surface-bound active antimicrobials, biocidal coatings, and passive pathogen-repellent surfaces, developed using nanomaterials, chemical modifications, and micro- and nano-structuring. Nanomaterials are a prime candidate for such a solution. Here, we developed mesoporous silica nanoparticles (MSNs) loaded with antimicrobially active silver and copper ions that can be used in sprayable formulations as surface coatings. The influence of different surface functionalization and metal ion loadings on the efficacy of these sprayable coatings was studied. Amine- (MSN-NH2), carboxy- (MSN-COOH) and thiol-functionalized mesoporous silica nanoparticles (MSN-SH) were synthesized and characterized using different techniques, such as transmission electron microscopy (TEM), attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), dynamic light scattering (DLS), electrophoretic light scattering (Zeta potential measurements) and nitrogen sorption measurements. After loading MSNs with antimicrobially active silver or copper ions, the nanoparticle dispersions were spray-coated on stainless steel substrates that were primed with sprayable polyelectrolyte solutions to enhance coating homogeneity and nanoparticle adhesion. The metal ion release was analyzed by Inductively coupled plasma optical emission spectroscopy (ICP-OES). The antimicrobial properties of the nanoparticle suspension and the coatings were tested against three commonly found pathogenic bacteria, Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli as well as a fungal pathogen, Candida albicans. The toxicity of the coatings against human skin cells was also assessed. T2 - STOP Antimicrobial Coatings Conference CY - Mons, Belgium DA - 05.12.2024 KW - Mesoporous Silica Nanoparticles KW - Antimicrobial Coatings KW - Spray-Coating KW - Pathogens PY - 2024 AN - OPUS4-62180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruehle, Bastian T1 - Natural language processing for automated workflow and knowledge graph generation in self-driving labs N2 - Natural language processing with the help of large language models such as ChatGPT has become ubiquitous in many software applications and allows users to interact even with complex hardware or software in an intuitive way. The recent concepts of Self-Driving Labs and Material Acceleration Platforms stand to benefit greatly from making them more accessible to a broader scientific community through enhanced user-friendliness or even completely automated ways of generating experimental workflows that can be run on the complex hardware of the platform from user input or previously published procedures. Here, two new datasets with over 1.5 million experimental procedures and their (semi)automatic annotations as action graphs, i.e., structured output, were created and used for training two different transformer-based large language models. These models strike a balance between performance, generality, and fitness for purpose and can be hosted and run on standard consumer-grade hardware. Furthermore, the generation of node graphs from these action graphs as a user-friendly and intuitive way of visualizing and modifying synthesis workflows that can be run on the hardware of a Self-Driving Lab or Material Acceleration Platform is explored. Lastly, it is discussed how knowledge graphs – following an ontology imposed by the underlying node setup and software architecture – can be generated from the node graphs. All resources, including the datasets, the fully trained large language models, the node editor, and scripts for querying and visualizing the knowledge graphs are made publicly available. KW - Natural Language Processing KW - Large Language Models KW - Self-Driving Labs KW - Materials Acceleration Platforms KW - Workflows KW - Nanomaterials KW - Advanced Materials PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631947 UR - https://github.com/BAMresearch/MAPz_at_BAM/tree/main/Minerva-Workflow-Generator DO - https://doi.org/10.1039/d5dd00063g SN - 2635-098X SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zaki, Mohammad T1 - Nano- And Advanced Materials Synthesis In A Self-driving Lab (SDL) N2 - Development of new nano- and advanced materials - or improvement of existing ones - are important drivers in materials research due to the high importance of these material classes for various applications. Traditional laboratory methods for material development often suffer from reproducibility issues, inefficiencies, human errors, and long experimental optimization times. To overcome these challenges and thus accelerate and optimize the process of material synthesis and discovery, we are building a Self-Driving Lab (SDL), in which we integrate robotics for autonomous nanomaterial synthesis, and automated characterization and data analysis for a complete and reliable nanomaterial synthesis workflow. We also leverage artificial intelligence (AI) and machine learning (ML) algorithms to analyze characterization results and plan new experiments to optimize material properties in an ML-guided active learning feedback loop. Our SDL is very agnostic towards the types of nano- and advanced materials it can synthesize. On the same SDL platform, we successfully synthesized Stober silica, mesoporous silica, copper-oxide, and gold nanoparticles, as well as metal-organic frameworks and more complex structures from multi-step reactions, such as Au@SiO2 and CuO@SiO2 core-shell nanoparticles. All these material syntheses showed excellent reproducibility when run on the SDL platform multiple times. Automated, in-line characterization measurements of hydrodynamic diameter, zeta potential, and optical properties (absorbance, fluorescence) of the nanomaterials have also been incorporated in the SDL, along with automating data analysis of at-line or off-line characterization techniques such as electron microscopy image analyses [1]. Incorporating these characterization results alongside a machine learning feedback loop that suggests new experimental parameters for obtaining materials with target properties is a key step for developing autonomous, closed-loop optimization processes. In such a process, we typically start by using random sampling to suggest initial experimental parameters, followed by ML-guided active learning algorithms such as Bayesian optimization, artificial neural networks, or downhill simplex optimizers (e.g., Nelder-Mead) that suggest new synthesis parameters to finally arrive at a material with the targeted or enhanced properties. Further improvement and optimization of our SDL has the potential to mitigate challenges faced by traditional approaches and open a way for rapid and reproducible nano- and advanced material synthesis, optimization, and discovery. T2 - ANAKON Conference 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Self-driving laboratories KW - Materials acceleration platforms KW - Nanomaterials KW - Advanced materials KW - Automation KW - Robotics KW - In-line characterization PY - 2025 AN - OPUS4-62737 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data acquisition system for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution N2 - This study presents our data acquisition system prototype for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution (nanoDAQ) and a matching data processing approach for time-resolved data in the nanosecond range. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. Particle-by-particle-based analysis of ion event density and other parameters derived from nanosecond time resolution show promising results. High data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leaves only the sample uptake and rinsing steps as remaining factors for limiting the total measurement time. T2 - 20th European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization PY - 2025 AN - OPUS4-63599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - Workflow generation, management, and semantic description for Self-Driving Labs N2 - The software backend that controls the robotic hardware and runs the synthesis workflows is a very important component of any Self-Driving Lab (SDL). On the one hand, it has to deal with orchestrating and managing complex and task-specific hardware through low-level communication protocols and plan and use the available resources as efficiently as possible while executing (parallelized) workflows, on the other hand, it is the interface the users use to communicate with this highly complex platform, and as such, it needs to be as helpful and user-friendly as possible. This includes the AI-aided experimental design in which the system helps the user to decide which experiment to run next, providing automated data analysis from characterization measurements, and offering easy to understand tools and graphical user interfaces for generating the workflows that are executed on the platform. Lastly, the specificity of the workflows and their dependence on the hardware and software of the SDLs necessitates a common description or ontology for making them easily interchangeable and interoperable between different platforms and labs. In this contribution, we present several key aspects of “Minerva-OS”, the central backend that orchestrates the syntheses workflows of our SDL for Nano- and Advanced Materials Syntheses [1]. One key feature is the resource management or “traffic control” for scheduling and executing parallel reactions in a multi-threaded environment. Another is the interface with data analysis algorithms from in-line, at-line, and off-line measurements. Here, we will give examples of how automatic image segmentation of electron microscopy images with the help of AI [2] can be used for reducing the “data analysis bottleneck” from an off-line measurement. We will also discuss, compare, and show benchmarks of various machine learning (ML) algorithms that are currently implemented in the backend and can be used for ML-guided, closed-loop material optimization in our SDL. Lastly, we will show our recent efforts [3] in making the workflow generation on SDLs more user-friendly by using large language models to generate executable workflows automatically from synthesis procedures given in natural language and user-friendly graphical user interfaces based on node editors that also allow for knowledge graph extraction from the workflows. In this context, we are currently also working on an ontology for representing the process steps of the workflows, which will greatly facilitate the semantic description and interoperability of workflows between different SDL hardware and software platforms. T2 - Accelerate 2025 CY - Toronto, Canada DA - 11.08.2025 KW - Nanomaterials KW - Advanced Materials KW - Workflows KW - Machine Learning KW - SDL PY - 2025 AN - OPUS4-63936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - Nano- and Advanced Materials Synthesis in a Self-Driving Lab (SDL) N2 - Nano- and advanced materials have been recognized as a key enabling technology of the 21st century, due to their high potential of driving innovations in new clean energy technologies, sustainable manufacturing by substitution of critical raw materials and replacement of hazardous substances, breakthroughs in energy conversion and storage, improvement of the environmental performance of products and processes, and facilitation of circularity. Consequently, improving tools that enhance the development and optimization cycle of nano- and advanced materials is crucial. In this contribution, we present our Self-Driving Lab (SDL) for Nano and Advanced Materials [1], that integrates robotics for batched autonomous synthesis – from molecular precursors to fully purified nanomaterials – with automated characterization and data analysis, for a complete and reliable nanomaterial synthesis workflow. By fully automating these three process steps for seven different materials from five representative, completely different classes of nano- and advanced materials (metal, metal oxide, silica, metal organic framework, and core–shell particles) that follow different reaction mechanisms, we demonstrate the great versatility and flexibility of the platform. The system also exhibits high modularity and adaptability in terms of reaction scales and incorporates in-line characterization measurement of hydrodynamic diameter, zeta potential, and optical properties (absorbance, fluorescence) of the nanomaterials. We discuss the excellent reproducibility of the various materials synthesized on the platform in terms of particle size and size distribution, and the adaptability and modularity that allows access to a diverse set of nanomaterial classes. These features underscore the SDL’s potential as a transformative tool for advancing and accelerating the development of nano- and advanced materials, offering solutions for a sustainable and environmentally responsible future. T2 - Accelerate 2025 CY - Toronto, Canada DA - 11.08.2025 KW - Nanomaterials KW - Advanced Materials KW - Automation KW - SDL KW - MAP PY - 2025 AN - OPUS4-63935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - Nano- and Advanced Materials Synthesis in a Self-Driving Lab (SDL) N2 - Nano- and advanced materials have been recognized as a key enabling technology of the 21st century, due to their high potential of driving innovations in new clean energy technologies, sustainable manufacturing by substitution of critical raw materials and replacement of hazardous substances, breakthroughs in energy conversion and storage, improvement of the environmental performance of products and processes, and facilitation of circularity. Consequently, improving tools that enhance the development and optimization cycle of nano- and advanced materials is crucial. In this contribution, we present our Self-Driving Lab (SDL) for Nano and Advanced Materials [1], that integrates robotics for batched autonomous synthesis – from molecular precursors to fully purified nanomaterials – with automated characterization and data analysis, for a complete and reliable nanomaterial synthesis workflow. By fully automating these three process steps for seven different materials from five representative, completely different classes of nano- and advanced materials (metal, metal oxide, silica, metal organic framework, and core–shell particles) that follow different reaction mechanisms, we demonstrate the great versatility and flexibility of the platform. The system also exhibits high modularity and adaptability in terms of reaction scales and incorporates in-line characterization measurement of hydrodynamic diameter, zeta potential, and optical properties (absorbance, fluorescence) of the nanomaterials. We discuss the excellent reproducibility of the various materials synthesized on the platform in terms of particle size and size distribution, and the adaptability and modularity that allows access to a diverse set of nanomaterial classes. These features underscore the SDL’s potential as a transformative tool for advancing and accelerating the development of nano- and advanced materials, offering solutions for a sustainable and environmentally responsible future. T2 - Accelerate 2025 CY - Toronto, Canada DA - 11.08.2025 KW - Nanomaterials KW - Advanced Materials KW - Automation KW - SDL KW - MAP PY - 2025 AN - OPUS4-63934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vermeeren, Sarah A1 - Witzler, Markus A1 - Makarow, Ramona A1 - Engelhard, Carsten A1 - Kaul, Peter T1 - Multivariate evaluation method for the detection of pest infestations on plants via VOC analysis using gas chromatography mass spectrometry N2 - Volatile organic compounds (VOCs) play an important role in the defense against pest infestations on plants. The analysis of these VOCs using gas chromatography mass spectrometry (GC-MS) enables the detection of pests by analyzing the VOC composition (VOC profiles) for specific patterns and markers. The analysis of such complex datasets with high biovariability poses a particular challenge. For this reason, a multivariate evaluation method based on a self-written Python script, using principal component analysis (PCA) and linear discriminant analysis (LDA), was developed and tested for functionality using a dataset, which has been evaluated manually and has identified five specific markers (2,4-dimethyl-1-heptene, 3-carene, alpha-longipinene, cyclosativene, and copaene) for Anoplophora glabripennis (ALB) infestation on Acer trees. The results obtained in the present study did not only match the manually evaluated results, but lead to further insight into the dataset. Another sesquiterpene which is assumed to be alpha-zingiberene was identified as an ALB specific marker in addition to 2,4-dimethyl-1-heptene and 3-carene. Furthermore, the European native beetle species goat moth Cossus cossus (CC) and poplar long-horned beetle Saperda carcharias (SC) were also analyzed for their VOCs to differentiate ALB specific VOC from other pest infestations. This comparison lead to the conclusion that the compounds alpha-longipinene, cyclosativene, and copaene are not specific for ALB but for pest infestation in general. It was possible to identify not only specifically produced VOCs, but also differences in concentrations that arise specifically during ALB infestation. Therefore, the evaluation method for the detection of plant pests presented in this study represents a time-saving alternative to conventional non computing methods, which in addition provides more detailed results. KW - Mass Spectrometry KW - Gas Chromatography KW - Volatile organic compounds KW - Pest infestation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639526 DO - https://doi.org/10.1038/s41598-025-11607-5 SN - 2045-2322 VL - 15 IS - 1 SP - 1 EP - 10 PB - Springer Science and Business Media LLC AN - OPUS4-63952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Jennifer A1 - Engelhard, Carsten A1 - Kaul, Peter T1 - Optimized fast gas chromatography coupled with proton-transfer-reaction time-of-flight mass spectrometry for the selective near real-time analysis of herbivore-induced plant volatiles N2 - The analysis of herbivore-induced plant volatiles (HIPVs) is essential for understanding plant-environment interactions and defense strategies against herbivores. Proton transfer reaction time-of-flight mass spectrometry (PTR–TOF–MS) is a powerful analytical tool that enables real-time monitoring and quantification of diverse groups of HIPVs. However, the PTR–TOF–MS technique is constrained in its ability to effectively differentiate between isomers. When analyzing complex mixtures of HIPVs, the separation of isomers becomes crucial as major compound classes such as terpenes comprise thousands of isomers. In this study, we present an optimized fast gas chromatography (fastGC) based on a modified version of the commercially available fastGC add-on integrated into a mobile PTR–TOF. The system was optimized for the analysis of emissions from enclosed trunks of Acer platanoides infested by Anoplophora glabripennis (Motschulsky), commonly known as Asian longhorned beetle (ALB). The development of fastGC was primarily focused on the sesquiterpenes α-longipinene, cyclosativene and α-copaene, which serve as strong indicators of ALB infestation. These sesquiterpenes were separated in less than three minutes, with intra-day retention time RSD < 0.6 % and resolutions of 2.6 ± 0.3 and 1.3 ± 0.2. In comparison to the original system, the optimized fastGC demonstrates more than tripled sesquiterpene resolution, twice the sensitivity relative to direct inlet mode, and an approximately 10 % reduction in total analysis time. The optimized fastGC–PTR–TOF allows for near real-time analysis of complex mixtures of biogenic VOCs, making it a powerful tool for environmental monitoring, integrated pest management, and forest protection. KW - Mass Spectrometry KW - PTR-TOF-MS KW - Gas Chromatography KW - Herbivore-induced plant volatiles KW - Sesquiterpenes PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639513 DO - https://doi.org/10.1016/j.chroma.2025.466236 SN - 0021-9673 VL - 1759 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-63951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Bestimmung von Spurenstoffen im (Roh-)Abwasser mittels ELISA N2 - Der Vortrag behandelt die Bestimmung von Spurenstoffen im Rohabwasser mithilfe von ELISA (Enzyme-Linked Immunosorbent Assay), einer immunanalytischen Methode, die sich durch hohe Sensitivität und Eignung für Hochdurchsatzanalysen auszeichnet. Im Rahmen der Projekte MARKERIA I & II wurden verschiedene anthropogene Marker wie Koffein, Carbamazepin, Diclofenac, Bisphenol A und Hormone wie Östron untersucht, um deren Eignung für die Abwassersurveillance zu bewerten. Die Ergebnisse zeigen, dass einige Substanzen wie Carbamazepin stabile Konzentrationen aufweisen und sich gut als Marker eignen, während andere wie Koffein starke Schwankungen zeigen. Einige Marker wie Isolithocholsäure werden zwar in hohen Konzentrationen gefunden, zeigen aber methodische Herausforderungen wie instabile Assays. Die Studie hebt hervor, dass es Hotspots mit erhöhten Konzentrationen gibt, aber insgesamt eine relativ geringe Variabilität zwischen verschiedenen Rohabwässern besteht. Zukünftige Entwicklungen sollen sich auf die Verbesserung von Antikörpern, die Entwicklung tragbarer Vor-Ort-Analysemethoden und die Standardisierung immunanalytischer Verfahren konzentrieren. T2 - AMELAG-Colloquium "Spurenstoffe im (Ab-)Wasser" CY - Online meeting DA - 20.06.2025 KW - Antikörper KW - Schnelltests KW - Abwasser KW - ELISA PY - 2025 AN - OPUS4-63500 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Xinyue A1 - Dong, Ximan A1 - Zhang, Chuyan A1 - Zhu, Meng A1 - Ahmed, Essraa A1 - Krishnamurthy, Giridharan A1 - Rouzbahani, Rozita A1 - Pobedinskas, Paulius A1 - Gauquelin, Nicolas A1 - Jannis, Daen A1 - Kaur, Kawaljit A1 - Hafez, Aly Mohamed Elsayed A1 - Thiel, Felix A1 - Bornemann, Rainer A1 - Engelhard, Carsten A1 - Schönherr, Holger A1 - Verbeeck, Johan A1 - Haenen, Ken A1 - Jiang, Xin A1 - Yang, Nianjun T1 - Interlayer Affected Diamond Electrochemistry N2 - Diamond electrochemistry is primarily influenced by quantities of sp3‐carbon, surface terminations, and crystalline structure. In this work, a new dimension is introduced by investigating the effect of using substrate‐interlayers for diamond growth. Boron and nitrogen co‐doped nanocrystalline diamond (BNDD) films are grown on Si substrate without and with Ti and Ta as interlayers, named BNDD/Si, BNDD/Ti/Si, and BNDD/Ta/Ti/Si, respectively. After detailed characterization using microscopies, spectroscopies, electrochemical techniques, and density functional theory simulations, the relationship of composition, interfacial structure, charge transport, and electrochemical properties of the interface between diamond and metal is investigated. The BNDD/Ta/Ti/Si electrodes exhibit faster electron transfer processes than the other two diamond electrodes. The interlayer thus determines the intrinsic activity and reaction kinetics. The reduction in their barrier widths can be attributed to the formation of TaC, which facilitates carrier tunneling, and simultaneously increases the concentration of electrically active defects. As a case study, the BNDD/Ta/Ti/Si electrode is further employed to assemble a redox‐electrolyte‐based supercapacitor device with enhanced performance. In summary, the study not only sheds light on the intricate relationship between interlayer composition, charge transfer, and electrochemical performance but also demonstrates the potential of tailored interlayer design to unlock new capabilities in diamond‐based electrochemical devices. KW - Nanocrystalline diamond KW - Interfaces KW - Electrochemistry KW - TOF-SIMS KW - SEM PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621576 DO - https://doi.org/10.1002/smtd.202301774 SN - 2366-9608 VL - 9 IS - 2 SP - 1 EP - 10 PB - Wiley VHC-Verlag CY - Weinheim AN - OPUS4-62157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelhard, Carsten T1 - On ICP-MS with Nanosecond Time Resolution: From Nanoparticles to Microplastics N2 - In this presentation, recent developments in inductively coupled plasma mass spectrometry (ICP-MS) instrumentation for particle characterization in complex mixtures will be reviewed. The current state-of-the-art in single-particle (sp) ICP-MS instrumentation for the detection and characterization of nanoparticles (NP) and microplastics (MPs) as well as remaining challenges will be discussed. While millisecond dwell times were used in the advent of spICP-MS, the use of microsecond dwell times helped to improve nanoparticle data quality and particle size detection limits. We could show that a custom-built high-speed data acquisition unit with microsecond time resolution (μsDAQ) can be used to successfully address issues of split-particle events and particle coincidence, to study the temporal profile of individual ion clouds, and to extend the linear dynamic range by compensating for dead time related count losses. Our latest development is an in-house built data acquisition system with nanosecond time resolution (nanoDAQ). Recording of the SEM signal by the nanoDAQ is performed on the nanosecond time scale with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. In addition to inorganic nanoparticles, first results on the detection of microplastics with spICP-MS will be discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Nano KW - Microplastics KW - Nanoparticle Characterization KW - ICP-MS KW - Instrumentation PY - 2025 AN - OPUS4-63580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelhard, Carsten T1 - From Particles to PFAS: Recent Advances in Plasma-based Instrumentation Development N2 - In this presentation, recent advances in plasma spectrochemistry with hot and cold plasma sources for the direct detection of nanoparticles as well as per- and polyfluoroalkyl substances (PFAS) will be discussed. In the first part, single-particle inductively coupled plasma mass spectrometry (spICP-MS) with an in-house built data acquisition system with nanosecond time resolution (nanoDAQ) will be presented. In the second part, we turn to a cooler plasma source. Specifically, a flowing atmospheric-pressure afterglow source (FAPA) and its application for the direct mass spectrometric analysis of PFAS will be discussed. T2 - 20th European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization KW - PFAS PY - 2025 AN - OPUS4-63581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Escobar-Carranza, Cristian C. T1 - On the Detection of Microplastics by Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (FAPA-MS) N2 - Microplastics (MPs) are widespread pollutant particles that can be analyzed using Raman and FTIR spectroscopy combined with optical microscopy. Additionally, pyrolysis (Py) or thermal extraction and desorption (TED) coupled with gas chromatography-mass spectrometry (GC-MS) are used for the characterization of MPs.[1] However, sample throughput is limited due to GC separation. This work presents a feasibility study for the direct, rapid analysis of MPs using high-resolution mass spectrometry and a plasma-based ambient desorption/ionization source (FAPA, flowing atmospheric-pressure afterglow).[2] In earlier work, an in-house built ambient ionization source (modelled after the pin-to-capillary (p2c) FAPA design by Shelley et al. [3]) was coupled to HR-Orbitrap MS and used to characterize different MPs produced in-house from plastic materials including polystyrene (PS), polypropylene (PP), low-density polyethylene (LDPE), and polycarbonate (PC). Simultaneous detection of characteristic ions and particle imaging on a sampling mesh was feasible, with detection limits (LOD) for PS MPs at 311 µm in size and 1.3 mg in mass. Principal component analysis (PCA) was used for particle differentiation. This work presents an improved desorption/ionization approach using higher temperatures for desorption enhancement (approximately 500 °C, achieved with economical and commercially available parts) and a tailored source housing combined with a halo-shaped (h-FAPA) source configuration.[4] The scope was expanded to include MPs from poly(ethylene terephthalate) (PET), poly(methyl methacrylate) (PMMA), and poly(vinyl chloride) (PVC), sized 125–250 µm. Data visualization and interpretation were performed using Kendrick mass defect plots and other multivariate analysis tools. Compared to earlier results, h-FAPA-MS yielded at least 65% higher ion signals for selected ions in all MPs. These ions were detected mainly as protonated species [M+H]+. Higher thermal desorption temperatures aided in detecting all MPs, as the presence of higher molecular weight fragments added specificity to the analysis. Notably, experiments with the h-FAPA source demonstrated lower mass-based LODs for MPs than the p2c-FAPA source (e.g., 14 µg vs 1.3 mg for PS, respectively). T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass Spectrometry KW - Plasma KW - FAPA-MS KW - Microplastics PY - 2025 AN - OPUS4-63604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schütz, Désirée A.-M. T1 - Feasibility Study on the Adsorption of Environmental Contaminants onto Fresh and Aged Microplastics N2 - Microplastics (MPs) refer to plastic particles, fibers, or beads with sizes ranging from 100 nm to 5 mm in size. Their pervasive distribution as environmental contaminants have escalated into a significant global concern. Primary MPs are intentionally produced particles for industrial and commercial applications, such as exfoliants in personal care and cosmetic formulations. In contrast, secondary MPs are generated through the fragmentation and degradation of larger plastic materials, due to environmental weathering processes. [1] Due to their high surface area-to-volume ratio and hydrophobic nature, MPs have the potential to serve as vectors for the accumulation and transport of diverse organic contaminants, including polycyclic aromatic hydrocarbons (PAHs), perfluoroalkyl substances (PFAS), pharmaceuticals and personal care products (PPCPs), as well as trace metals such as silver, cadmium, chromium, and copper. In the environmental, MPs are subject to aging processes driven by factors such as temperature, ultraviolet radiation, oxygen, and chemical interactions with environmental toxins. This aging can induce significant alterations in their physicochemical properties, which, in turn, can affect the adsorption behavior. [2] Classical and alternative analytical methods such as high-performance liquid chromatography (HPLC) and ambient desorption/ionization high-resolution mass spectrometry (ADI-HR-MS) can help to study the adsorption potential. ADI-HR-MS allows rapid sample analysis with minimal preparation, providing results in under a minute, much faster than traditional chromatographic techniques. [3] This study aims to investigate the influence of aging and particle size on the ability of microplastics to act as vectors for environmental contaminants. Microplastics were prepared in-house and subjected to controlled aging conditions for 12, 24, 36, and 48 hours. Subsequently, the aged MPs were exposed in plastic-free containers to model solutions to simulate co-contaminants in the environment. Adsorption onto synthesized secondary microplastics, varying in size and aging status, was investigated at different time intervals with ambient MS and time-of-flight secondary ion mass spectrometry. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass Spectrometry KW - FAPA-MS KW - Microplastics KW - TOF-SIMS KW - Surface Analysis PY - 2025 AN - OPUS4-63606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data acquisition system for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution N2 - This study presents our data acquisition system prototype for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution (nanoDAQ) and a matching data processing approach for time-resolved data in the nanosecond range. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. [1] Particle-by-particle-based analysis of ion event density and other parameters derived from nanosecond time resolution show promising results. High data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leaves only the sample uptake and rinsing steps as remaining factors for limiting the total measurement time. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization PY - 2025 AN - OPUS4-63603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chan, George C.-Y. A1 - Hieftje, Gary M. A1 - Omenetto, Nicoló A1 - Axner, Ove A1 - Bengtson, Arne A1 - Bings, Nicolas H. A1 - Blades, Michael W. A1 - Bogaerts, Annemie A1 - Bolshov, Mikhail A. A1 - Broekaert, José A.C. A1 - Chan, WingTat A1 - Costa-Fernández, José M. A1 - Crouch, Stanley R. A1 - De Giacomo, Alessandro A1 - D’Ulivo, Alessandro A1 - Engelhard, Carsten A1 - Falk, Heinz A1 - Farnsworth, Paul B. A1 - Florek, Stefan A1 - Gamez, Gerardo A1 - Gornushkin, Igor B. A1 - Günther, Detlef A1 - Hahn, David W. A1 - Hang, Wei A1 - Hoffmann, Volker A1 - Jakubowski, Norbert A1 - Karanassios, Vassili A1 - Koppenaal, David W. A1 - Kenneth Marcus, R. A1 - Noll, Reinhard A1 - Olesik, John W. A1 - Palleschi, Vincenzo A1 - Panne, Ulrich A1 - Pisonero, Jorge A1 - Ray, Steven J. A1 - Resano, Martín A1 - Russo, Richard E. A1 - Scheeline, Alexander A1 - Smith, Benjamin W. A1 - Sturgeon, Ralph E. A1 - Todolí, José-Luis A1 - Tognoni, Elisabetta A1 - Vanhaecke, Frank A1 - Webb, Michael R. A1 - Winefordner, James D. A1 - Yang, Lu A1 - Yu, Jin A1 - Zhang, Zhanxia T1 - Landmark Publications in Analytical Atomic Spectrometry: Fundamentals and Instrumentation Development N2 - The almost-two-centuries history of spectrochemical analysis has generated a body of literature so vast that it has become nearly intractable for experts, much less for those wishing to enter the field. Authoritative, focused reviews help to address this problem but become so granular that the overall directions of the field are lost. This broader perspective can be provided partially by general overviews but then the thinking, experimental details, theoretical underpinnings and instrumental innovations of the original work must be sacrificed. In the present compilation, this dilemma is overcome by assembling the most impactful publications in the area of analytical atomic spectrometry. Each entry was proposed by at least one current expert in the field and supported by a narrative that justifies its inclusion. The entries were then assembled into a coherent sequence and returned to contributors for a round-robin review. KW - Analytical atomic spectrometry KW - Spectroscopy KW - Instrumental analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621588 DO - https://doi.org/10.1177/00037028241263567 SN - 1943-3530 VL - 78 SP - 1 EP - 456 PB - Sage CY - London AN - OPUS4-62158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Tuma, Dirk A1 - Khanipour, Peyman A1 - Maiwald, Michael T1 - Voll normal - Normen in der Gasanalytik N2 - In dieser Arbeit werden die Grundlagen der Normung, die Entstehung einer Norm und die für die Gasanalytik relevanten Normungsgremien kurz dargestellt. Dazu werden die wichtigsten Normen zur Gasanalytik entlang des analytischen Prozesses gruppiert und aufgeführt. Schließlich wird als Anwendungsbeispiel aus der eigenen Praxis der Prozess von der Herstellung bis zur Zertifizierung eines Kalibriergases beschrieben. KW - Zertifikat KW - Regel- und Messtechnik KW - Normung KW - Gasanalytik KW - Gasgualität KW - Gasreinheit PY - 2022 SN - 2366-9594 VL - 10 SP - 73 EP - 80 PB - Vulkan Verlag CY - Essen AN - OPUS4-56083 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinelt, Manuel T1 - Feasibility Study on the Direct Detection of Per- and Polyfluoroalkyl Substances (PFAS) with Surface-Assisted Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (SA-FAPA-MS) N2 - Per- and polyfluoroalkyl substances (PFAS) are a large class of thousands of synthetic chemicals that are used worldwide. However, growing environmental and human health concerns in the last two decades have led to more stringent regulatory requirements and the development of quantitative analytical methods for PFAS detection. Today, standardized and powerful methods exist, e.g., for the determination of PFAS in water, sludge, compost, soil, and drinking water (DIN 38407-42, DIN 38414-14, ISO 21675, and DIN EN 17892). While liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) is often used, blank levels, sample preparation, and total analysis times can be challenging. [1] Here, ambient desorption/ionization mass spectrometry (ADI-MS) is considered interesting because it requires only minimal sample preparation and was able to reduce total analysis time in other types of applications. [2] Previously, we used a plasma-based pin-to-capillary flowing atmospheric-pressure afterglow source (FAPA) [3] to probe samples directly from thin-layer chromatography (TLC) plates and to perform quantitative analysis and mass spectral imaging [4]. In this work, a feasibility study for the direct detection of PFAS with FAPA-MS is reported. Selected PFAS samples were directly probed on functionalized TLC surfaces (normal-phase silica, reversed-phase-modified silica, cyano [CN]-modified silica, and dimethyl [RP2]-modified silica, diol modified silica, and amino [NH2]-modified silica). The suitability of the surfaces was evaluated and the compatibility of different solvents with the surfaces was studied. CN-HPTLC and RP2-TLC surfaces showed the best performance for direct PFAS detection with FAPA-MS. In addition, direct analysis of PFAS mixtures and selected matrices was performed with little sample preparation and short analysis time. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass Spectrometry KW - FAPA-MS KW - Instrumentation KW - PFAS KW - Surface Analysis PY - 2025 AN - OPUS4-63605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinelt, Manuel T1 - Feasibility Study on the Direct Detection of Per- and Polyfluoroalkyl Substances (PFAS) with Surface-Assisted Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (SA-FAPA-MS) N2 - Per- and polyfluoroalkyl substances (PFAS) are a large class of thousands of synthetic chemicals that are used worldwide. However, growing environmental and human health concerns in the last two decades have led to more stringent regulatory requirements and the development of quantitative analytical methods for PFAS detection. Today, standardized and powerful methods exist, e.g., for the determination of PFAS in water, sludge, compost, soil, and drinking water (DIN 38407-42, DIN 38414-14, ISO 21675, and DIN EN 17892). While liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) is often used, blank levels, sample preparation, and total analysis times can be challenging. [1] Here, ambient desorption/ionization mass spectrometry (ADI-MS) is considered interesting because it requires only minimal sample preparation and was able to reduce total analysis time in other types of applications. [2] Previously, we used a plasma-based pin-to-capillary flowing atmospheric-pressure afterglow source (FAPA) [3] to probe samples directly from thin-layer chromatography (TLC) plates and to perform quantitative analysis and mass spectral imaging [4]. In this work, a feasibility study for the direct detection of PFAS with FAPA-MS is reported. Selected PFAS samples were directly probed on functionalized TLC surfaces (normal-phase silica, reversed-phase-modified silica, cyano [CN]-modified silica, and dimethyl [RP2]-modified silica, diol modified silica, and amino [NH2]-modified silica). The suitability of the surfaces was evaluated and the compatibility of different solvents with the surfaces was studied. CN-HPTLC and RP2-TLC surfaces showed the best performance for direct PFAS detection with FAPA-MS. In addition, direct analysis of PFAS mixtures and selected matrices was performed with little sample preparation and short analysis time. T2 - 56th Annual Conference of the DGMS CY - Göttingen, Germany DA - 04.03.2025 KW - FAPA-MS KW - Instrumentation KW - Mass Spectrometry KW - PFAS KW - Surface Analysis PY - 2025 AN - OPUS4-63643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schütz, Désirée A.-M. T1 - Feasibility Study on the Adsorption of Environmental Contaminants onto Fresh and Aged Microplastics N2 - Microplastics (MPs) refer to plastic particles, fibers, or beads with sizes ranging from 100 nm to 5 mm in size. Their pervasive distribution as environmental contaminants have escalated into a significant global concern. Primary MPs are intentionally produced particles for industrial and commercial applications, such as exfoliants in personal care and cosmetic formulations. In contrast, secondary MPs are generated through the fragmentation and degradation of larger plastic materials, due to environmental weathering processes. [1] Due to their high surface area-to-volume ratio and hydrophobic nature, MPs have the potential to serve as vectors for the accumulation and transport of diverse organic contaminants, including polycyclic aromatic hydrocarbons (PAHs), perfluoroalkyl substances (PFAS), pharmaceuticals and personal care products (PPCPs), as well as trace metals such as silver, cadmium, chromium, and copper. In the environmental, MPs are subject to aging processes driven by factors such as temperature, ultraviolet radiation, oxygen, and chemical interactions with environmental toxins. This aging can induce significant alterations in their physicochemical properties, which, in turn, can affect the adsorption behavior. [2] Classical and alternative analytical methods such as high-performance liquid chromatography (HPLC) and ambient desorption/ionization high-resolution mass spectrometry (ADI-HR-MS) can help to study the adsorption potential. ADI-HR-MS allows rapid sample analysis with minimal preparation, providing results in under a minute, much faster than traditional chromatographic techniques. [3] This study aims to investigate the influence of aging and particle size on the ability of microplastics to act as vectors for environmental contaminants. Microplastics were prepared in-house and subjected to controlled aging conditions for 12, 24, 36, and 48 hours. Subsequently, the aged MPs were exposed in plastic-free containers to model solutions to simulate co-contaminants in the environment. Adsorption onto synthesized secondary microplastics, varying in size and aging status, was investigated at different time intervals with ambient MS and time-of-flight secondary ion mass spectrometry. T2 - 56th Annual Conference of the DGMS CY - Göttingen, Germany DA - 04.03.2025 KW - FAPA-MS KW - Mass Spectrometry KW - Microplastics KW - Surface Analysis KW - TOF-SIMS PY - 2025 AN - OPUS4-63644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schardt, Annika T1 - Fast screening method for nanoparticles in surface waters via nanosecond spICP-MS and a tailored automated ion cloud recognition algorithm N2 - Single particle inductively coupled plasma mass spectrometry (spICP-MS) is a powerful technique for nanoparticle (NP) analysis in aqueous samples, which provides essential information on size distribution and particle number concentration (PNC) of nanometer-sized particles in various water samples for risk assessment and toxicity tests. In contrast to spectroscopic particle analysis methods, this mass spectrometry-based tool can provide chemical information on the elemental composition of NPs after minimal sample preparation. We recently presented a novel spICP-MS instrumentation and tailored software that acquires data with nanosecond time resolution, lowering the particle size detection limit to 7 nm for gold NP (1). The system directly samples the output signal of the electron multiplier and records the detection of individual ions with a time resolution of only a few nanoseconds. With nanosecond time resolution, we were able to visualize profiles of ion clouds that were produced from ionization of nanoparticles in the ICP on a single-ion basis and to use the temporal gap between those ions for particle sizing. Our latest improvement of the data acquisition system (nanoDAQ) features ca. 2 ns integration time and a matching processing software prototype, which automatically recognizes and counts ion clouds in the transient data. With this combination we achieved an experimentally determined size detection limit of ca. 5 nm for gold nanoparticles. A feasibility study shows that the nanoDAQ in combination with the ion cloud recognition algorithm succeeds in fast detection and counting of NP containing Ag, Ce, or Zr in waste water and surface water samples from the area of Siegen. PNCs ranged from ca. 7 x 106–2 x 108 particles/L, which is in good agreement with concentrations reported for similar water samples in the literature. T2 - 56th Annual Conference of the German Society for Mass Spectrometry (DGMS) CY - Göttingen, Germany DA - 04.03.2025 KW - Instrumentation KW - Mass Spectrometry KW - Nanoparticles KW - spICP-MS PY - 2025 AN - OPUS4-63662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Escobar-Carranza, Cristian C. T1 - On the Detection of Microplastics by Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (FAPA-MS) N2 - Microplastics (MPs) are widespread pollutant particles analyzed using Raman and FTIR spectroscopy combined with optical microscopy. Pyrolysis (Py) or thermal extraction and desorption (TED) coupled with gas chromatography-mass spectrometry (GC-MS) are used for the characterization of MPs, though GC limits sample throughput. This work explores direct, rapid MP analysis using high-resolution (HR) MS and a plasma-based ambient desorption/ionization source (FAPA, flowing atmospheric-pressure afterglow). Previously, an in-house pin-to-capillary (p2c) FAPA source coupled to HRMS characterized MPs made in-house from polystyrene (PS), polypropylene (PP), low-density polyethylene (LDPE), and polycarbonate (PC). Simultaneous detection of characteristic ions and particle imaging on a sampling mesh was feasible, with detection limits (LOD) for PS MPs at 311 µm in size and 1.3 mg in mass. Principal component analysis (PCA) was used for particle differentiation. This work introduces a high-temperature desorption method (~500 °C) with economical and commercially available parts and a tailored housing combined with a halo-shaped (h-FAPA) source configuration. The study expands to include poly(ethylene terephthalate) (PET), poly(methyl methacrylate) (PMMA), and poly(vinyl chloride) (PVC) MPs (125–250 µm). Data visualization and interpretation were performed using Kendrick mass defect plots and other multivariate analysis tools. Compared to earlier results, h-FAPA-MS yielded at least 65% higher ion signals for selected ions in all MPs. These ions were detected mainly as protonated species [M+H]+. Higher thermal desorption temperatures aided in detecting all MPs, as the presence of higher molecular weight fragments added specificity to the analysis. Notably, experiments with the h-FAPA source demonstrated lower mass-based LODs for MPs than the p2c-FAPA source (e.g., 14 µg vs 1.3 mg for PS, respectively). T2 - 56th Annual Conference of the German Society for Mass Spectrometry (DGMS) CY - Göttingen, Germany DA - 04.03.2025 KW - Instrumentation KW - Mass Spectrometry KW - FAPA-MS KW - Microplastics PY - 2025 AN - OPUS4-63663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oskoei, P. A1 - Nogueira, J. A1 - Keller, Lisa-Marie A1 - Andresen, Elina A1 - Maturi, F. E. A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Daniel-da-Silva, A. L. A1 - Carlos, L. D. A1 - Oliviera, H. T1 - Effects of doxorubicin-loaded UCNP@MSN core-shell particles with a thermoresponsive nanovalve in melanoma cells N2 - Melanoma, one of the most aggressive forms of skin cancer, has an increasingly higher incidence. When detected in advanced stages, tumour eradication is often incomplete, contributing to poor prognosis with conventional treatments. Upconversion nanoparticles (UCNPs) haveunique optical properties that allow their effective use in several biomedical applications. This includes the excitability under near-infrared (NIR) excitation light, which has a relatively high penetration depth in tissue, a multitude of characteristic emission bands in the ultraviolet (UV), visible (Vis), NIR, and short-wave infrared (SWIR), along with long luminescence lifetimes, and high photostability. Mesoporous silica nanoparticles (MSN) with nanovalves or derived coatings have widely been used for triggered and targeted drug delivery in the past. Anticancer drugs can be loaded into the pores of MSN, enabling spatiotemporally controlled drug release. KW - Nano KW - Particle KW - Silica KW - Upconversation KW - Lanthanide KW - Triggered release KW - Temperature KW - Cell studies KW - Drug KW - Toxicity studies PY - 2024 DO - https://doi.org/10.1016/j.toxlet.2024.07.237 SN - 0378-4274 VL - 399 IS - Supplement 2 SP - S89 EP - S90 PB - Elsevier B.V. AN - OPUS4-62571 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oskoei, Parastu T1 - Thermoresponsive UCNP@MSN Nanoparticles for Doxorubicin Delivery in Melanoma Cells N2 - Upconversion nanoparticles (UCNPs) possess unique photophysical characteristics, such as excita bility by near infrared (NIR) light, which facilitates deep tissue penetration, multi color emission , long luminescence lifetimes, and an excellent photostability. These features have made UCNPs promising tools for biomedical applications . M esoporous silica nanoparticles (MSNs) functionalized with stimuli responsive nanovalves or specific coatings enable the encapsulation and controlled release of therapeutic agen ts, thereby offering spatiotemporal precision in drug delivery 1 3 ]]. Among drug delivery strategies, photoresponsive systems have attracted growing attention due to their potential for clinical applications . This is especially relevant for melanoma, an aggressive skin cancer with increasing global incidence, for which conventional therapeutic modalities remain largely insufficient in advanced stage 4 In this work, core shell UCNP@MSN nanoparticles were synthetised by coating UCNPs with a mesoporous silica layer, which was subsequently functionalized with thermoresponsive retro Diels Alder nanovalves [ and loaded with the chemotherapeutic agent doxorubicin (DOX). Controlled drug release was effectively achieved under 980 nm NIR i llumination . Treatment with functionalized nanoparticles significantly reduced the viability of melanoma cell lines, with an enhanced cytotoxicity being observed upon combined nanoparticle exposure and NIR illumination . Mechanistic analyses revealed that neither UCNPs nor NIR i llumination alone could induce the production of reactive oxygen species (ROS); however, their combination induced a marked increase in ROS levels in two of the three tested cell lines. Furthermore, this dual treatment promoted substantial apoptotic and/or necrotic responses across all cell models. These findings underscore the potential of UCNP@MSN nanoplatforms, equipped with thermoresponsive ga tes , as efficient photoactivated drug delivery systems for melanoma therapy. T2 - Conference Jornadas CICECO CY - Aveiro, Portugal DA - 09.10.2025 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 - OPUS4-64371 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 - Oskoei, Párástu T1 - Effects of upconversion nanoparticles with a thermo-responsive nanovalve loaded with doxorubicin in melanoma cells N2 - Melanoma skin cancer has an increasingly higher incidence , and w hen detected in advanced stages, tumour eradication is often incomplete, contributing to poor prognosis with conventional treatments. Upconversion nanoparticles (UCNPs) have unique properties, such as excitability under near infrared (NIR) excitation light, which confers a relatively high penetration depth in tissue that allow their effective use in several biomedical applications Mesoporous silica nanoparticles (MSN) with nanovalves or derived coatings have widely been used for triggered and targeted drug delivery in the past. Anticancer drugs can be loaded into the pores of MSN, enabling controlled drug release. In this work, UCNPs were coated with a mesoporous silica shell yielding UCNP@MSN core shell nanoparticles which were equipped with thermoresponsive retro Diels Alder nanovalves and then loaded with DOX , a chemotherapeutic agent for melanoma treatmen t (UCNP@MSN DOX) Subsequent DOX release from this drug delivery system was triggered by 980 nm NIR light. Melanoma cells exposed to UCNP@MSN DOX or the NIR laser exhibited no change in ROS production , while the combination of both induced an increase in ROS production. This combination of conditions also induced changes on apoptosis and necrosis levels. These findings underscore the potential use of UCNP @MSN drug delivery systems with thermoresponsive caps as effective drug delivery platforms for melanoma therapy. T2 - VII iBiMED Symposium CY - Aveiro, Portugal DA - 23.05.2025 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 - OPUS4-64373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heide, Maximilian A1 - Reifenrath, Jonas A1 - Herrmann, Alexander A1 - Engelhard, Carsten T1 - Fast and Sustainable Active Pharmaceutical Ingredient (API) Screening in Over-the-Counter and Prescription Drug Products by Surface-Assisted Plasma-Based Desorption/Ionization High-Resolution Mass Spectrometry N2 - Fast chemical analysis of pharmaceutical preparations is important for quality assurance, counterfeit drug detection, and consumer health. While quantitative methods such as high-performance liquid chromatography mass spectrometry (HPLC-MS) are powerful, there is a need for sustainable and environmentally friendly methods, which require less chemicals and produce less waste. Here, solvent-free ambient desorption/ionization (ADI) MS methods are attractive because they do not require time-consuming chromatography, produce little to no chemical waste, and, thus, contribute to green chemistry practice. In addition, sample throughput can be higher compared to HPLC-MS. In this study, a method for direct analysis of single- and multi agent drugs using a plasma-based ADI source (flowing atmospheric-pressure afterglow, FAPA) coupled to high-resolution (HR) MS was developed and optimized for best performance. The approach is rapid and only requires analytes to be in solution (only a few µL) before application onto thin-layer chromatography (TLC) surfaces, specifically dimethyl (RP2-) and cyano (CN-) modified silica, for surface-assisted (SA) FAPA-HRMS measurements. No chromatographic separation was required, and the TLC plates served only as sample carriers. A broad variety of 19 active pharmaceutical ingredients (APIs) was carefully selected to cover analgesics, anesthetics, antibiotics, antiepileptics, calcium channel blockers, diuretics, expectorants, opioids, peripheral vasodilators, stimulants, and sympathomimetics. Fast screening and identification of APIs was performed by SA-FAPA-HRMS. Typically, the protonated molecular ion ([M+H]+) was the most abundant species, while some compounds (codeine, metamizole, phenoxymethylpenicillin, and torasemide) did show some degree of fragmentation. As a proof-of-principle application, benzocaine was directly detected in saliva samples post-intake of a lozenge. Time-resolved semi-quantitative screening was performed. The limit of detection for benzocaine in saliva was 8 ng/mL (48.4 fmol) using internal standard calibration and CN-HPTLC plates. In addition, direct quantification of artificially spiked saliva was performed with minimal sample preparation. Here, SA-FAPA-HRMS with a CN-HPTLC sample substrate yielded best performance (20.02±0.52 µg/mL, RSD=2.6%, deviation of -1.9% from the theoretical value) compared to RP2-TLC (18.97±1.37 µg/mL, RSD=7.2%, -7.0%), and HPLC-UV (18.51±0.03 µg/mL, RSD=0.2%, -9.3%) results. In conclusion, SA FAPA HRMS is considered attractive for rapid and sustainable analysis of pharmaceuticals with potential in non-invasive patient monitoring. KW - Mass Spectrometry KW - Pharmaceuticals KW - Green Chemistry KW - Ambient Desorption/Ionization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640718 DO - https://doi.org/10.1039/D5AY01050K SN - 1759-9660 VL - 17 IS - 18 SP - 7799 EP - 7809 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - The potential of Material Acceleration Platforms (MAPs) for creating resilient and sustainable technology value chains N2 - Material Acceleration Platforms (MAPs) represent a transformative approach to the development of resilient and sustainable technology value chains. These platforms can identify candidate chemistries and structures via simulations, and database searches and leverage machine learning-based rapid screening to accelerate the discovery and deployment of novel materials, thereby addressing critical challenges in modern technology sectors. Incorporating high-fidelity advanced characterization in the early phases of material development is crucial for early de-risking. Advanced characterization techniques, such as X-ray diffraction, advanced electrochemical and spectroscopic techniques provide comprehensive insights into the structural, chemical, and physical properties of materials. Long-term testing further contributes to the de-risking process by evaluating the durability and stability of materials under various environmental and operational conditions. Early identification of potential degradation mechanisms enables the refinement of material compositions and processing methods, ultimately leading to the development of more resilient materials. Early upscaling attempts are integral to assessing the feasibility of material leads generated through machine learning-based rapid screening to evaluate the scalability of synthesis and processing techniques. This step is critical for identifying potential challenges in manufacturing, such as issues related to reproducibility, yield, and cost-effectiveness. Process design has to be a major part of the MAP-based material design to cope with the increasing share of secondary raw materials in supply chains. This presentation will briefly summarize possible strategies to address these issues and provide deep-dives on best practices. As the demand for advanced materials continues to grow, MAPs will play an increasingly vital role in driving technological advancements and addressing global challenges. T2 - Materials Week Cyprus 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - MAPs KW - SDLs KW - Sustainability PY - 2024 AN - OPUS4-60379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - A Self-Driving Lab for Nano and Advanced Materials Synthesis N2 - Nano- and advanced materials have been recognized as a key enabling technology of the 21st century, due to their high potential of driving innovations in new clean energy technologies, sustainable manufacturing by substitution of critical raw materials and replacement of hazardous substances, breakthroughs in energy conversion and storage, improvement of the environmental performance of products and processes, and facilitation of circularity. Consequently, new tools that enhance the development and optimization cycle of nano- and advanced materials are crucial. In this contribution, we present our Self-Driving Lab (SDL) for Nano and Advanced Materials [1], that integrates robotics for batched autonomous synthesis – from molecular precursors to fully purified nanomaterials – with automated characterization and data analysis, for a complete and reliable nanomaterial synthesis workflow. By fully automating the processing steps for seven different materials from five representative, completely different classes of nano- and advanced materials (metal, metal oxide, silica, metal organic framework, and core–shell particles) that follow different reaction mechanisms, we demonstrate the great versatility and flexibility of the platform. The system also exhibits high modularity and adaptability in terms of reaction scales and incorporates in-line characterization measurement of hydrodynamic diameter, zeta potential, and optical properties (absorbance, fluorescence). We discuss the excellent reproducibility of the various materials synthesized on the platform in terms of particle size and size distribution, and the adaptability and modularity that allows access to a diverse set of nanomaterial classes. We also present several key aspects of the central backend that orchestrates the (parallelized) syntheses workflows. One key feature is the resource management or “traffic control” for scheduling and executing parallel reactions in a multi-threaded environment. Another is the interface with data analysis algorithms from in-line, at-line, and off-line measurements. Here, we will give examples of how automatic image segmentation of electron microscopy images with the help of AI [2] can be used for reducing the “data analysis bottleneck” from an off-line measurement. We will also discuss various machine learning (ML) algorithms that are currently implemented in the backend and can be used for ML-guided, closed-loop material optimization in our SDL. Lastly, we will show our recent efforts [3] in making the workflow generation on SDLs more user-friendly by using large language models to generate executable workflows automatically from synthesis procedures given in natural language and user-friendly graphical user interfaces based on node editors that also allow for knowledge graph extraction from the workflows. In this context, we are currently also working on a common description or ontology for representing the process steps and parameters of the workflows, which will greatly facilitate the semantic description and interoperability of workflows between different SDL hardware and software platforms. These features underscore the SDL’s potential as a transformative tool for advancing and accelerating the development of nano- and advanced materials, offering solutions for a sustainable and environmentally responsible future. T2 - MRS Fall Meeting 2025 CY - Boston, MA, USA DA - 30.11.2025 KW - Self-Driving Labs KW - Materials Acceleration Platforms KW - Advanced Materials KW - Nanomaterials KW - Automation PY - 2025 AN - OPUS4-65129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayat, Mehmet E. A1 - Huber, C. A1 - Kipphardt, Heinrich A1 - Tiebe, Carlo A1 - Engelhard, Carsten T1 - Towards a sensor-based methodology to determine online calorific values of H2-enriched natural gases in the grid N2 - The German National Hydrogen Strategy (NWS) envisions a transition towards a hydrogen-based energy grid. However, due to the material incompatibility of existing pipeline infrastructure for amounts of hydrogen higher than 10 cmol/mol, many system components of the existing grid must be replaced with significant costs and considerable time investments. Given these constraints, the admixture of hydrogen into natural gas (NG) to create a hydrogen-enriched NG blend has been designated as a transitional technology. The NWS supports this approach on a regional and time-limited basis, but clearly states that it is not intended as a permanent solution. Nevertheless, the conversion to a fully hydrogen-based grid is expected to take several decades. During this transitional phase, precise process analytical monitoring of hydrogen amounts in the NG blend is essential to ensure both energy efficiency via calorific value control and operational safety. These procedures require cost-effective, robust, and reliable sensor technologies capable of real-time, in situ/on-site quantification of hydrogen amounts in NG. In response to this need, we have advanced a physical sensing approach utilizing an oscillating cantilever in collaboration with Truedyne Sensor AG. This sensor system enables quantification of hydrogen amounts, direct calorific value determination as well as display of beneficial gas properties, like density, viscosity, and thermal conductivity. Moreover, the enhanced cantilever system enables direct physical sensing and can also be operated in a quasi-binary mode. We performed comparative evaluations against two benchmark sensor systems to validate the developed technology. One utilizes chemical sensing, and the other operates on thermal conductivity measurements for hydrogen quantification. Through standardized testing, we demonstrated that the cantilever-based sensor offers both high effectiveness and competitive performance compared to current state-of-the-art technologies for accurate hydrogen detection in natural gas and precise determination of its calorific value. T2 - Gas Analysis 2026 CY - Paris, France DA - 27.01.2026 KW - Hydrogen KW - Natural Gas KW - Sensor KW - Calorific Value KW - Grid PY - 2026 AN - OPUS4-65505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaki, Mohammad A1 - Prinz, Carsten A1 - Ruehle, Bastian T1 - A Self-Driving Lab for Nano- and Advanced Materials Synthesis N2 - The recent emergence of self-driving laboratories (SDL) and material acceleration platforms (MAPs) demonstrates the ability of these systems to change the way chemistry and material syntheses will be performed in the future. Especially in conjunction with nano- and advanced materials which are generally recognized for their great potential in solving current material science challenges, such systems can make disrupting contributions. Here, we describe in detail MINERVA, an SDL specifically built and designed for the synthesis, purification, and in line characterization of nano- and advanced materials. By fully automating these three process steps for seven different materials from five representative, completely different classes of nano- and advanced materials (metal, metal oxide, silica, metal organic framework, and core–shell particles) that follow different reaction mechanisms, we demonstrate the great versatility and flexibility of the platform. We further study the reproducibility and particle size distributions of these seven representative materials in depth and show the excellent performance of the platform when synthesizing these material classes. Lastly, we discuss the design considerations as well as the hardware and software components that went into building the platform and make all of the components publicly available. KW - Self-driving laboratories KW - Materials acceleration platforms KW - Nanomaterials KW - Advanced materials KW - Automation KW - Robotics KW - In-line characterization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627361 DO - https://doi.org/10.1021/acsnano.4c17504 SN - 1936-086X VL - 19 IS - 9 SP - 9029 EP - 9041 PB - ACS Publications CY - Washington, DC AN - OPUS4-62736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Competence Center nano@BAM Welcomes ISO/TC 229 Meeting in Berlin N2 - The Competence Center nano@BAM is presented. Examples directly related to the activities of the ISO Technical Committee TC 229 Nanotechnologies as well as BAM projects on nano reference measurement procedures, nano reference materials and nano reference data sets are showed. T2 - The 32nd ISO/TC 229 IEC/TC 113 JWG2 General Meeting CY - Berlin, Germany DA - 06.11.2023 KW - ISO/TC 229 Nanotechnologies KW - Nanoparticles KW - Nano@BAM KW - Reference materials KW - Reference data KW - Reference procedures PY - 2023 AN - OPUS4-58814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Correlative analysis with electron microscopy applied in different operating modes (SEM, STEM-in-SEM and TEM) for the accurate morphological characterisation of non-spherical fine nanoparticles N2 - Electron microscopy applied in different operating modes, e.g., SEM, TEM or STEM-in-SEM, is the gold standard method to investigate the exact size and shape of individual nanoparticles. However, when fine nanoparticles with a non-monodisperse size distribution and non-spherical shapes are analysed, achieving an accurate result is challenging. Deviations in size measurements of more than 10% may occur. Understanding of the contrasts and sensitivities characteristic to the individual operating modes of an electron microscope is key in interpreting and evaluating quantitatively the measurement uncertainties needed for an eventual certification of specific nanoparticles via traceable results. Further, beyond the pure measurement, the other components in the analysis workflow with significant impact on the overall measurement uncertainties are the sample preparation and the image segmentation. In the present study the same areas of selected iron oxide fine nanoparticles (<25 nm) as reference nanomaterial (candidate) prepared on substrate for electron microscopy imaging are analysed correlatively with SEM, STEM-in-SEM and TEM with respect to their size and shape distribution. Individual significant measurement uncertainties are discussed, e.g., the sensitivity of secondary electron detectors of InLens-type to the surface morphology, particularly to the presence of an ultrathin organic coating or signal saturation effects on the particle edges, to electron beam exposure, to surface contamination, or the selection of the threshold for image segmentation. Another goal of this study is to establish a basis of analysis conditions which shall guarantee accurate results when both manual and particularly (semi-)automated segmentation approaches are applied. Advantages as well as limitations of the use of different electron microscopy operating modes, applied individually and correlatively, are highlighted. T2 - E-MRS 2024 Spring Meeting CY - Strasbourg, France DA - 27.05.2024 KW - Nanoparticles KW - Electron Microscopy KW - Metrology KW - Imaging KW - Reference materials PY - 2024 AN - OPUS4-60436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Hodoroaba, Vasile-Dan T1 - Understanding Correlative Electron Microscopy Imaging with SEM, STEM in SEM and TEM for the Accurate Characterization of Size and Shape of FeOx Nanoparticles N2 - The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM). For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary. The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM. With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically). ❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility. ❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs. ❑ Selection of the threshold algorithm can significantly alter the reported ECD. T2 - Microscopy and Microanalysis 2024 CY - Cleveland, OH, USA DA - 28.07.2024 KW - Nanoparticles KW - Electron microscopy KW - Iron oxide KW - Reference materials KW - Correlative microscopy KW - Size and shape distribution PY - 2024 AN - OPUS4-60806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Understanding Correlative Electron Microscopy Imaging with SEM, STEM-in-SEM and TEM for the Accurate Characterization of Size and Shape of FeOx Nanoparticles N2 - The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM). For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary. The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM. With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically). ❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility. ❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs. ❑ Selection of the threshold algorithm can significantly alter the reported ECD. T2 - SALSA Make and Measure 2024: Interfaces CY - Berlin, Germany DA - 11.09.2024 KW - Correlative microscopy KW - Electron microscopy KW - Iron oxide KW - Nanoparticles KW - Reference materials KW - Size and shape distribution PY - 2024 AN - OPUS4-62347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Understanding Correlative Electron Microscopy Imaging with SEM, STEM in SEM and TEM for the Accurate Characterization of Size and Shape of FeOx Nanoparticles N2 - The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM). For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary. The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM. With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically). ❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility. ❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs. ❑ Selection of the threshold algorithm can significantly alter the reported ECD T2 - 2. Treffen des DGE-Arbeitskreises SEM CY - Stuttgart, Germany DA - 26.09.2024 KW - Correlative microscopy KW - Electron microscopy KW - Iron oxide KW - Nanoparticles KW - Reference materials KW - Size and shape distribution PY - 2024 AN - OPUS4-62349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Thünemann, Andreas A1 - Rühle, Bastian A1 - Radnik, Jörg A1 - Bresch, Harald A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as Certified Reference Material for Size and Shape N2 - BAM is currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance to the material and life sciences. As a first candidate of this series, we present cubic iron oxide nanoparticles with a nominal edge length of 8 nm. These particles were synthesized by thermal decomposition of iron oleate in high boiling organic solvents adapting well-known literature procedures. After dilution to a concentration suitable for electron microscopy (TEM and SEM) as well as for small-angle X-ray scattering (SAXS) measurements, the candidate nanoRM was bottled and assessed for homogeneity and stability by both methods following the guidelines of ISO 17034 and ISO Guide 35. The particle sizes obtained by both STEM-in-SEM and TEM are in excellent agreement with a minimum Feret of 8.3 nm ± 0.7 nm. The aspect ratio (AR) of the iron oxide cubes were extracted from the images as the ratio of minimum Feret to Feret resulting in an AR of 1.18 for TEM to 1.25 for SEM. Alternatively, a rectangular bounding box was fitted originating from the minimum Feret and the longest distance through the particle in perpendicular direction. This led to AR values of 1.05 for TEM and 1.12 for SEM, respectively. The results confirm the almost ideal cubic shape. KW - Reference nanoparticles KW - Iron oxide KW - Cubical shape KW - Electron microscopy KW - SAXS KW - Nano CRM KW - Size PY - 2022 DO - https://doi.org/10.1017/S1431927622003610 SN - 1435-8115 VL - 28 IS - Suppl. 1 SP - 802 EP - 805 PB - Cambridge University Press AN - OPUS4-55599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Soraya A1 - Hülagü, Deniz A1 - Bennet, Francesca A1 - Carl, Peter A1 - Flemig, Sabine A1 - Schmid, Thomas A1 - Schenk, J. A. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf T1 - Electrochemical Immunomagnetic Ochratoxin A Sensing: Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine in Amperometric Assays N2 - Electrochemical methods offer great promise in meeting the demand for user-friendly on-site devices for Monitoring important parameters. The food industry often runs own lab procedures, for example, for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with smart technologies. Enzyme-linked immunosorbent assays, with photometric detection of 3,3’,5,5’-tetramethylbenzidine (TMB),form a good basis for sensitive detection. To provide a straightforward approach for the miniaturization of the detectionstep, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry it was found that the TMB electrochemistry is strongly dependent on the pH and the electrode material. A stable electrode response to TMB could be achieved at pH 1 on gold electrodes. We created a smartphonebased, electrochemical, immunomagnetic assay for the detection of ochratoxin A in real samples, providing a solid basis forsensing of further analytes. KW - Ochratoxin A KW - Amperometry KW - Cyclic voltammetry KW - Electrochemistry KW - Immunoassay PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530421 DO - https://doi.org/10.1002/celc.202100446 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. VL - 8 IS - 13 SP - 2597 EP - 2606 AN - OPUS4-53042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Rühle, Bastian A1 - Kuchenbecker, Petra A1 - Löhmann, Oliver A1 - Lindemann, Franziska A1 - Hodoroaba, Vasile-Dan T1 - Embedding and cross-sectioning as a sample preparation procedure for accurate and representative size and shape measurement of nanopowders N2 - Reliable measurement of the size of polydisperse, complex-shaped commercial nanopowders is a difficult but necessary task, e.g., for regulatory requirements and toxicity risk assessment. Suitable methods exist for the accurate characterization of the size of non-aggregated, stabilized, spherical and monodisperse nanoparticles. In contrast, industrial nanoscale powders usually require dedicated sample preparation procedures developed for the analysis method of choice. These nano-powders tend to agglomerate and/or aggregate, a behavior which in combination with an innate broad particle size distribution and irregular shape often significantly alters the achievable accuracy of the measured size parameters. The present study systematically tests two commercially available nanoscale powders using different sample preparation methods for correlative analysis by scanning electron microscopy, dynamic light scattering, Brunauer–Emmet–Teller method and differential mobility analysis. One focus was set on the sample preparation by embedding nanoparticles in carbon-based hot-mounting resin. Literature on this topic is scarce and the accuracy of the data extracted from cross sections of these particles is unclearly stated. In this paper systematic simulations on the deviation of the size parameters of well-defined series of nanoparticles with different shapes from the nominal value were carried out and the contributing factors are discussed. KW - Nanopowder KW - Electron microscopy KW - Sample preparation KW - Cross-sectioning KW - Cerium oxide KW - Zinc oxide PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593289 DO - https://doi.org/10.1038/s41598-023-51094-0 SN - 2045-2322 VL - 14 SP - 1 EP - 10 PB - Springer Nature CY - London AN - OPUS4-59328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Rühle, Bastian A1 - Hodoroaba, Vasile-Dan T1 - Understanding Correlative Electron Microscopy Imaging with SEM, STEM-in-SEM and TEM for the Accurate Characterization of Size and Shape of Iron Oxide Nanoparticles N2 - The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM). For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary. The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM. With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically). ❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility. ❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs. ❑ Selection of the threshold algorithm can significantly alter the reported ECD. KW - Nanoparticles KW - Iron oxide KW - Electron microscopy KW - Reference materials KW - Particle size distribution KW - Imaging PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.339 VL - 30 IS - Supplement_1 SP - 710 EP - 711 PB - Oxford University Press (OUP) AN - OPUS4-61007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Onyenso, Gabriel A1 - AI-Zawity, Jiwar A1 - Farahbakhsh, Nastaran A1 - Schardt, Annika A1 - Yadigarli, Aydan A1 - Vakamulla Raghu, Swathi Naidu A1 - Engelhard, Carsten A1 - Müller, Mareike A1 - Schönherr, Holger A1 - Killian, Manuela S. T1 - Novel Ag-modified zirconia nanomaterials with antibacterial activity N2 - The outcome of an implant procedure largely depends on the implant's surface properties. Biomaterials are now designed to have surfaces with multifunctionality, such as favorable tissue integration and the ability to combat bacterial adhesion and colonization. Herein, we report on a simple approach to improve the antibacterial properties of zirconia nanotubes (ZrNTs) coatings by decorating with silver nanoparticles (AgNP), achieved through electrochemical anodization of a zirconium–silver alloy (Zr–Ag). The AgNPs were shown to partially consist of Ag2O, potentially enhancing the availability of Ag+ ions for antibacterial activity. The modified ZrNTs were characterized using SEM, EDS, ToF-SIMS, and XPS to determine their structural morphology and chemical composition, and were further subjected to antibacterial testing. The silver and zirconium ion release behavior was monitored via ICP-MS. ZrNTs decorated with AgNP exhibit strong antimicrobial activity (>99% bacterial killing) against both S. aureus and E. coli. Antimicrobial tests indicate that the antibacterial activity against the Gram-positive pathogen S. aureus was improved by a factor of 100 compared to unmodified ZrNTs, while unmodified ZrNTs already showed a comparable reduction of viable Gram-negative E. coli. This strategy illustrates a straightforward and effective modification that optimizes the interface between the host environment and the biomaterial surface to meet the very important criteria of biocompatibility and active antibacterial response. KW - Mass Spectrometry KW - Nanoparticles KW - Advanced Materials KW - ICP-MS KW - Antimicrobial material KW - ToF-SIMS PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653990 DO - https://doi.org/10.1039/d5ra07099f SN - 2046-2069 VL - 16 IS - 3 SP - 2286 EP - 2297 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayat, Mehmet Emin A1 - Kipphardt, Heinrich A1 - Tiebe, Carlo A1 - Tuma, Dirk A1 - Engelhard, Carsten T1 - Trace-Level Ammonia–Water Interactions in Hydrogen: Challenges in Gas Purity Analysis Using Optical-Feedback Cavity-Enhanced Absorption Spectroscopy (OF-CEAS) N2 - Ammonia is a critical impurity in hydrogen fuel due to its irreversible poisoning effect on proton exchange membrane fuel cells. Therefore, international standards (e.g., ISO 14687) set a stringent threshold of 100 nmol/mol. Furthermore, with the growing potential use of ammonia as a hydrogen carrier, its accurate quantification is becoming increasingly important. However, the presence of trace humidity poses analytical challenges, as ammonia may interact with water or interfaces, thereby affecting its detectability. Therefore, the goal of this work is to enable accurate trace ammonia quantification for hydrogen purity measurements through fundamental studies of the methodological challenges. Here, low-pressure sampling (ultra)long-path Optical-Feedback Cavity-Enhanced Absorption Spectroscopy (OF-CEAS) was applied with an effective optical path length of approximately 6.17 km. We studied three average amounts of ammonia: (38.2 ± 0.8) nmol/mol, (74.8 ± 0.7) nmol/mol, and (112.1 ± 1.2) nmol/mol. Furthermore, these amounts were investigated at trace-humidity levels ranging from 0.8 to 8.5 ppmV. We observed a systematic, nonlinear, and humidity-dependent positive measurement bias of up to + (1.0 ± 0.2) nmol/mol at the maximum investigated trace-humidity volume fraction of 8.5 ppmV. This bias was not caused by spectral interference but rather by water-induced accumulation of ammonia within the optical cavity. Moreover, time-resolved measurements in the presence of trace ammonia showed that water desorption follows first-order kinetics, whereas water adsorption followed mixed-order kinetics with an apparent reaction order of 1.57 ± 0.03. Distinct hydration states of surface-bound ammonia were identified, whereas under dry conditions and with increasing amounts of ammonia, enhanced surface adhesion through intermolecular clustering was observed. In addition, the presence of ammonium species within the sorption layer was indirectly confirmed by our experiments. In conclusion, we provide a deeper insight into trace-level ammonia–water interactions and establish a framework for optimizing methodologies, particularly for (ultra)long-path optical gas measurement systems. KW - Ammonia KW - Hydrogen KW - OF-CEAS KW - Humidity KW - Surface Interactions KW - Adsorption PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643627 DO - https://doi.org/10.1021/acsmeasuresciau.5c00105 SN - 2694-250X SP - 1 EP - 15 PB - American Chemical Society (ACS) AN - OPUS4-64362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -