TY - JOUR A1 - Pavasarytė, Lina A1 - Azevedo do Nascimento, Allana A1 - Cysne Barbosa, Ana Paula A1 - Trappe, Volker A1 - Melo, Daniel T1 - Effects of particle size and particle concentration of poly (ethylene-co-methacrylic acid) on properties of epoxy resin N2 - Self-healing polymers have been developed to improve durability and reduce costs associated with maintenance during service. The addition of thermoplastics to thermosets to produce mendable polymers appears as a promising selfhealing technique. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was added to epoxy resin and the effects of EMAA addition on epoxy properties were evaluated. Specimens with two different contents of thermoplastic and particles sizes were manufactured. A two-level full factorial experimental design was used to evaluate the effect of particle size and particle content on properties of epoxy modified with addition of EMAA. Tensile tests and dynamic mechanical analysis (DMA) were used and the evaluated responses were tensile strength, modulus of elasticity, and glass transition temperature (Tg). X-ray computed tomography (XCT) was used to investigate particle size and concentration after manufacturing. It was found that the particle concentration has greater effects on stress–strain behavior of epoxy while Tg was not significantly affected by neither of the analyzed entrance variables. KW - Fracture KW - Self-healing KW - Epoxy KW - Thermoplastic PY - 2024 DO - https://doi.org/10.1002/app.55677 SN - 0021-8995 SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-60205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Groschke, Matthias A1 - Becker, Roland T1 - Comparison of carrier gases for the separation and quantification of mineral oil hydrocarbon (MOH) fractions using online coupled high performance liquid chromatography-gas chromatography-flame ionisation detection N2 - On-line coupled high performance liquid chromatography-gas chromatography-flame ionisation detection (HPLC-GC-FID) was used to compare the effect of hydrogen, helium and nitrogen as carrier gases on the chromatographic characteristics for the quantification of mineral oil hydrocarbon (MOH) traces in food related matrices. After optimisation of chromatographic parameters nitrogen carrier gas exhibited characteristics equivalent to hydrogen and helium regarding requirements set by current guidelines and standardisation such as linear range, quantification limit and carry over. Though nitrogen expectedly led to greater peak widths, all required separations of standard compounds were sufficient and humps of saturated mineral oil hydrocarbons (MOSH) and aromatic mineral oil hydrocarbons (MOAH) were appropriate to enable quantitation similar to situations where hydrogen or helium had been used. Slightly increased peak widths of individual hump components did not affect shapes and widths of the MOSH and MOAH humps were not significantly affected by the use of nitrogen as carrier gas. Notably, nitrogen carrier gas led to less solvent peak tailing and smaller baseline offset. Overall, nitrogen may be regarded as viable alternative to hydrogen or helium and may even extend the range of quantifiable compounds to highly volatile hydrocarbon eluting directly after the solvent peak. KW - Mineral oil hydrocarobons KW - Food KW - Liquid chromatography KW - Gas chromatography KW - MOSH/MOAH PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601450 DO - https://doi.org/10.1016/j.chroma.2024.464946 SN - 0021-9673 VL - 1726 SP - 1 EP - 7 PB - Elsevier CY - New York, NY AN - OPUS4-60145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Stephan A1 - Hoffmann, Holger A1 - Garbe, Leif-Alexander A1 - Harrer, Andrea A1 - Steiner, Markus A1 - Himly, Martin A1 - Schneider, Rudolf T1 - Re-assessment of monoclonal antibodies against diclofenac for their application in the analysis of environmental waters N2 - The non-steroidal anti-inflammatory drug (NSAID) diclofenac (DCF) is an important environmental contaminant occurring in surface waters all over the world, because, after excretion, it is not adequately removed from wastewater in sewage treatment plants. To be able to monitor this pollutant, highly efficient analytical methods are needed, including immunoassays. In a medical research project, monoclonal antibodies against diclofenac and its metabolites had been produced. Based on this monoclonal anti-DCF antibody, a new indirect competitive enzyme-linked immunosorbent assay (ELISA) was developed and applied for environmental samples. The introduction of a spacer between diclofenac and the carrier protein in the coating conjugate led to higher sensitivity. With a test midpoint of 3 mg L−1 and a measurement range of 1–30 mg L−1, the system is not sensitive enough for direct analysis of surface water. However, this assay is quite robust against matrix influences and can be used for wastewater. Without adjustment of the calibration, organic solvents up to 5%, natural organic matter (NOM) up to 10 mg L−1, humic acids up to 2.5 mg L−1, and salt concentrations up to 6 g L−1 NaCl and 75 mg L−1 CaCl2 are tolerated. The antibody is also stable in a pH range from 3 to 12. Cross-reactivity (CR) of 1% or less was determined for the metabolites 40-hydroxydiclofenac (40-OH-DCF), 5-hydroxydiclofenac (5-OH-DCF), DCF lactam, and other NSAIDs. Relevant cross-reactivity occurred only with an amide derivative of DCF, 6-aminohexanoic acid (DCF-Ahx), aceclofenac (ACF) and DCF methyl ester (DCF-Me) with 150%, 61% and 44%, respectively. These substances, however, have not been found in samples. Only DCF-acyl glucuronide with a cross-reactivity of 57% is of some relevance. For the first time, photodegradation products were tested for cross-reactivity. With the ELISA based on this antibody, water samples were analysed. In sewage treatment plant effluents, concentrations in the range of 1.9–5.2 mg L−1 were determined directly, with recoveries compared to HPLC-MS/MS averaging 136%. Concentrations in lakes ranged from 3 to 4.4 ng L−1 and were, after pre-concentration, determined with an average recovery of 100% KW - Antikörper KW - Immunoassay KW - Wasser PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602280 DO - https://doi.org/10.1039/d3ay01333b VL - 16 IS - 21 SP - 3349 EP - 3363 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-60228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, Michael A1 - Oelze, Marcus A1 - Frick, Daniel A. A1 - Di Rocco, Tommaso A1 - Liesegang, Moritz A1 - Stuff, Maria A1 - Wiedenbeck, Michael T1 - Silicon and oxygen isotope fractionation in a silicified carbonate rock N2 - Silicon isotope fractionation during silicification is poorly understood and impedes our ability to decipher paleoenvironmental conditions from Si isotopes in ancient cherts. To investigate isotope fractionation during silica-for-carbonate replacement we analyzed the microscale Si and O isotope composition in different silica phases in a silicified zebra dolostone as well as their bulk δ18O and Δ’17O compositions. The subsequent replacement of carbonate layers is mimicked by decreasing δ18O and δ30Si. The textural relationship and magnitude of Si and O isotope fractionation is best explained by near-quantitative silica precipitation in an open system with finite Si. A Rayleigh model for silicification suggests positive Ɛ30/28Si during silicification, conforming with predictions for isotope distribution at chemical equilibrium from ab-initio models. Application of the modelled Ɛ30Si-T relationship yields silicification temperatures of approx. 50°C. To reconcile the δ18Ochert composition with these temperatures, the δ18O of the fluid must have been between -2.5 and -4 ‰, compositions for which the quartz phases fall close to the oxygen equilibrium fractionation line in three-isotope space. Diagenetic silica replacement appears to occur in O and Si isotopic equilibrium allowing reconstructions of temperatures of silicification from Si isotopes and derive the δ18O composition of the fluid – a highly desired value needed for accurate reconstructions of the temperature- and δ18O histories of the oceans. KW - Silicon isotopes PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603430 DO - https://doi.org/10.1016/j.chemgeo.2024.122120 SN - 0009-2541 VL - 658 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-60343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krone, David A1 - Esche, Erik A1 - Skiborowski, Mirko A1 - Repke, Jens-Uwe T1 - Optimization-based process synthesis by phenomena-based building blocks and an MINLP framework featuring structural screening N2 - An existing approach for optimization-based process synthesis with abstracted phenomena-based building blocks (PBB) is extended by implementing it into a novel MINLP framework with structural screening. Consistency across the multilayer MINLP framework is guaranteed by creating a MathML/XML data model and subsequently exporting the code to the different program parts. The novel framework focuses both on fidelity by implementing thermodynamically sound models and on generality by employing a state-space superstructure that spans a large search space. In order to retain tractability, we insert a structural screening layer which prescreens based on binary decision variables of the superstructure by graph- and rule-based analyses, penalizing non-physical instances without solution of the underlying MINLP. The MINLP framework is successfully applied on two challenging synthesis tasks to determine the separation of the feed streams of benzene and toluene, as well as of n-pentane, n-hexane, and n-heptane utilizing superstructures with two, respectively four PBB. KW - Process synthesis KW - Superstructure optimization KW - Distillation KW - Mathematical programming KW - Structural screening PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621955 DO - https://doi.org/10.1016/j.compchemeng.2024.108955 VL - 194 SP - 1 EP - 19 PB - Elsevier Ltd. AN - OPUS4-62195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tukhmetova, Dariya A1 - Langhammer, Nicole A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Online Isotope Analysis of Sulfur in Proteins via Capillary Electrophoresis Coupled With Multicollector ICP‐MS (CE/MC‐ICP‐MS): A Proof of Concept Study N2 - Isotope ratio analysis of sulfur in biological samples using inductively coupled plasma-mass spectrometry (ICP-MS) has gained significant interest for applications in quantitative proteomics. Advancements like coupling separation techniques with multicollector ICP-MS (MC-ICP-MS) enhance the throughput of species-specific sulfur isotope ratio measurements, fostering new avenues for studying sulfur metabolism in complex biological matrices. This proof-of-concept study investigates the feasibility of online CE/MC-ICP-MS for directly analyzing sulfur isotope ratios in proteins (albumin). Leveraging our previous work on the applicability of CE/ICP-MS for quantifying sulfur-containing biological molecules, we explore its potential for sulfur isotope analysis. Our results demonstrate that direct analysis of sulfur isotopes in albumin protein using online capillary electrophoresis MC-ICP-MS (CE/MC-ICP-MS) eliminates the need for laborious pretreatment steps, while yielding isotope ratios comparable to the reference values. Although initial precision can be improved through further system optimization and protein injection techniques, this approach paves the way for future analysis of mixtures of various biological compounds in, for example, clinical diagnosis studies. KW - Isotope analysis KW - Sulfur KW - CE/MC-ICP-MS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612439 DO - https://doi.org/10.1002/elps.202400128 SN - 0173-0835 SP - 1 EP - 6 PB - Wiley-Blackwell CY - Weinheim AN - OPUS4-61243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duddi, M. A1 - Kocherla, Amarteja A1 - Subramaniam, K. V. L. T1 - Evaluation of boundary and material influences on the dynamic electromechanical impedance response of the embedded PZT sensor in concrete N2 - The article explores the material and structural size effects on the electrical impedance response of the embedded PZT sensors which are used as an sensors/actuator in the smart sensing concrete. An embedded sensor for use in concrete monitoring is developed using Lead Zirconate Titanate (PZT). The electrical impedance (EI) response of the sensor placed inside concrete cubes of varying sizes are recorded for an applied electrical input of varying frequency. The dynamic response of the embedded PZT sensor to the applied electrical input is determined by the mechanical impedance offered by the surrounding medium. In specimens of finite size, the mechanical impedance to the motion of the PZT is influenced by the combination of dynamic material resistance and structural stiffness (size of the structure). The current study examined the effects of material resistance and size of structure on the EI response of the PZT sensor embedded in concrete medium. The influence of the size of the medium from small-sized specimens is seen in the form of secondary peaks, identified as structural peaks, on the resonance spectrum of the embedded PZT sensor. The structural peaks on the EI response are very dominant in the concrete cube of small sizes. Magnitude and intensity of these structural peaks attenuate with an increase in the size of the concrete cube. Also, the EI response from the smaller-sized specimens registered a significant leftward shift in the spectrum. The observations from the numerical simulations also showed the mechanical impedance of the surrounding concrete medium to the motion of the PZT also increases and converges at 150 mm. At sizes below 150 mm, the structural effects that are influenced by the specimen boundary must be separated to access the material properties of the concrete medium from the measured EI response of an embedded PZT sensor. At sizes, larger than 150 mm, the dynamic motion of the PZT patch and the measured EI response of the PZT patch depend only on the dynamic material properties of the concrete medium around the sensor. The zone of influence and its importance in standardization of PZT sensor for SHM of concrete structures is discussed. KW - PZT KW - Concrete sensor KW - Embedded KW - Electrical impedance KW - Mechanical impedance KW - Zone of influence PY - 2023 DO - https://doi.org/10.1016/j.sna.2023.114575 SN - 0924-4247 SN - 1873-3069 VL - 361 SP - 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-61791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dhull, N. A1 - Kaur, Gurpreet A1 - Jindal, K. A1 - Verma, M. A1 - Tomar, M. T1 - Microfluidics integrated NiO based electrolyte-gated FETs for the detection of cortisol N2 - A microfluidics integrated EGFET has been devised using NiO for the detection of cortisol. A low detection limit of 0.5 fg mL−1 has been achieved and human salivary cortisol has been successfully assessed. KW - Microfluidic system KW - Field effect transistor (FET) KW - Electrolyte gating PY - 2022 DO - https://doi.org/10.1039/d2tb01652d SN - 2050-7518 VL - 10 IS - 44 SP - 9226 EP - 9234 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-61772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Yue A1 - Colnaghi, Timoteo A1 - Gong, Yilun A1 - Zhang, Huaide A1 - Yu, Yuan A1 - Wei, Ye A1 - Gan, Bin A1 - Song, Min A1 - Marek, Andreas A1 - Rampp, Markus A1 - Zhang, Siyuan A1 - Pei, Zongrui A1 - Wuttig, Matthias A1 - Ghosh, Sheuly A1 - Körmann, Fritz A1 - Neugebauer, Jörg A1 - Wang, Zhangwei A1 - Gault, Baptiste T1 - Machine learning‐enabled tomographic imaging of chemical short‐range atomic ordering N2 - In solids, chemical short‐range order (CSRO) refers to the self‐organization of atoms of certain species occupying specific crystal sites. CSRO is increasingly being envisaged as a lever to tailor the mechanical and functional properties of materials. Yet quantitative relationships between properties and the morphology, number density, and atomic configurations of CSRO domains remain elusive. Herein, it is showcased how machine learning‐enhanced atom probe tomography (APT) can mine the near‐atomically resolved APT data and jointly exploit the technique's high elemental sensitivity to provide a 3D quantitative analysis of CSRO in a CoCrNi medium‐entropy alloy. Multiple CSRO configurations are revealed, with their formation supported by state‐of‐the‐art Monte‐Carlo simulations. Quantitative analysis of these CSROs allows establishing relationships between processing parameters and physical properties. The unambiguous characterization of CSRO will help refine strategies for designing advanced materials by manipulating atomic‐scale architectures. KW - Chemical short-range order (CSRO) KW - Atom probe tomography (APT) KW - Machine learning PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623777 DO - https://doi.org/10.1002/adma.202407564 SN - 1521-4095 VL - 36 IS - 44 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-62377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arıkan, Muzaffer A1 - Demir, Tuğçe Kahraman A1 - Yıldız, Zeynep A1 - Nalbantoğlu, Özkan Ufuk A1 - Korkmaz, Nur Damla A1 - Yılmaz, Nesrin H. A1 - Şen, Aysu A1 - Özcan, Mutlu A1 - Muth, Thilo A1 - Hanoğlu, Lütfü A1 - Yıldırım, Süleyman T1 - Metaproteogenomic analysis of saliva samples from Parkinson's disease patients with cognitive impairment N2 - Cognitive impairment (CI) is very common in patients with Parkinson’s Disease (PD) and progressively develops on a spectrum from mild cognitive impairment (PD-MCI) to full dementia (PDD). Identification of PD patients at risk of developing cognitive decline, therefore, is unmet need in the clinic to manage the disease. Previous studies reported that oral microbiota of PD patients was altered even at early stages and poor oral hygiene is associated with dementia. However, data from single modalities are often unable to explain complex chronic diseases in the brain and cannot reliably predict the risk of disease progression. Here, we performed integrative metaproteogenomic characterization of salivary microbiota and tested the hypothesis that biological molecules of saliva and saliva microbiota dynamically shift in association with the progression of cognitive decline and harbor discriminatory key signatures across the spectrum of CI in PD. We recruited a cohort of 115 participants in a multi-center study and employed multi-omics factor analysis (MOFA) to integrate amplicon sequencing and metaproteomic analysis to identify signature taxa and proteins in saliva. Our baseline analyses revealed contrasting interplay between the genus Neisseria and Lactobacillus and Ligilactobacillus genera across the spectrum of CI. The group specific signature profiles enabled us to identify bacterial genera and protein groups associated with CI stages in PD. Our study describes compositional dynamics of saliva across the spectrum of CI in PD and paves the way for developing non-invasive biomarker strategies to predict the risk of CI progression in PD. KW - Cognitive impairment (CI) KW - Parkinson’s disease (PD) KW - Metaproteogenomic analysis KW - Saliva sample PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624228 DO - https://doi.org/10.1038/s41522-023-00452-x SN - 2055-5008 VL - 9 IS - 1 SP - 1 EP - 10 PB - Nature Publ. Group CY - London AN - OPUS4-62422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kozachynskyi, Volodymyr A1 - Hoffmann, Christian A1 - Esche, Erik T1 - Why fixing alpha in the NRTL model might be a bad idea – Identifiability analysis of binary vapor-liquid equilibria N2 - New vapor-liquid equilibrium (VLE) data are continuously being measured and new parameter values, e.g., for the nonrandom two-liquid (NRTL) model are estimated and published. The parameter α, the nonrandomness parameter of NRTL, is often not estimated but is heuristically fixed to a constant value based on the involved components. This can be seen as a manual application of a (subset selection) regularization method. In this work, the practical parameter identifiability of the NRTL model for describing the VLE is analyzed. It is shown that fixing α is not always a good decision and sometimes leads to worse prediction properties of the final parameter estimates. Popular regularization techniques are compared and Generalized Orthogonalization is proposed as an alternative to this heuristic. In addition, the sequential Optimal Experimental Design and Parameter Estimation (sOED-PE) method is applied to study the influence of the regularization methods on the performance of the sOED-PE loop. KW - NRTL KW - VLE KW - Nonlinear programming KW - Model-based optimal experimental design PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623605 DO - https://doi.org/10.1016/j.ces.2024.121122 VL - 305 SP - 1 EP - 18 PB - Elsevier Ltd. AN - OPUS4-62360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bosc-Bierne, Gaby A1 - Weller, Michael G. T1 - Investigation of impurities in peptide pools T1 - Untersuchung von Verunreinigungen in Peptidpools N2 - Peptide pools are important research tools in different biomedical fields. They consist of a complex mixture of defined peptides, which places high demands on the production and quality control of these products. Previously it has been shown that the combination of UHPLC with high-resolution mass-spectrometry (HRMS) is a fast and powerful method to confirm the relative concentration and the structural identity of all peptides expected to be in the pool. In this work, the additional information contained in the UV chromatograms and mass spectra is used to search for impurities due to synthesis by-products and degradation during storage and transportation and to identify possible analytical artifacts. It was shown that most impurities are only present in trace amounts and can be considered uncritical for most applications. The most frequent and perhaps unexpected impurities were homo- and heterodimers caused by the free cysteines contained in these peptide pools. Furthermore, pyroglutamate and aspartimide formation, deamidation, methionine oxidation, and amino acid deletions could be found. This list is not intended to be comprehensive, but rather a brief guide to quickly identify impurities and, in the long term, to suggest possible changes in the composition of the peptide pools to avoid such impurities by design or by special precautions. N2 - Peptidpools sind wichtige Forschungsinstrumente in verschiedenen biomedizinischen Bereichen. Sie bestehen aus einer komplexen Mischung definierter Peptide, was hohe Anforderungen an die Herstellung und Qualitätskontrolle dieser Produkte stellt. In der Vergangenheit wurde gezeigt, dass die Kombination von UHPLC mit hochauflösender Massenspektrometrie (HRMS) eine schnelle und leistungsfähige Methode zur Bestätigung der relativen Konzentration und der strukturellen Identität aller Peptide ist, die in dem Pool erwartet werden. In dieser Arbeit werden die zusätzlichen Informationen, die in den UV-Chromatogrammen und Massenspektren enthalten sind, genutzt, um nach Verunreinigungen zu suchen, die auf Nebenprodukte der Synthese und den Abbau während der Lagerung und des Transports zurückzuführen sind, und um mögliche analytische Artefakte zu identifizieren. Es hat sich gezeigt, dass die meisten Verunreinigungen nur in Spuren vorhanden sind und für die meisten Anwendungen als unkritisch angesehen werden können. Die häufigsten und vielleicht unerwartetsten Verunreinigungen waren Homo- und Heterodimere, die durch die in diesen Peptidpools enthaltenen freien Cysteine verursacht werden. Außerdem wurden Pyroglutamat- und Aspartimidbildung, Deamidierung, Methioninoxidation und Aminosäuredeletionen festgestellt. Diese Liste erhebt keinen Anspruch auf Vollständigkeit, sondern ist eher ein kurzer Leitfaden, um Verunreinigungen schnell zu identifizieren und langfristig mögliche Änderungen in der Zusammensetzung der Peptidpools vorzuschlagen, um solche Verunreinigungen durch Design oder besondere Vorsichtsmaßnahmen zu vermeiden. KW - Synthetic peptides KW - Degradation KW - Synthetic artifacts KW - Peptide losses KW - Stability of peptides KW - Disulfide dimers KW - Cysteine dimers KW - Isomers KW - Cysteine alkylation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626987 DO - https://doi.org/10.3390/separations12020036 SN - 2297-8739 VL - 12 IS - 2 SP - 1 EP - 18 PB - MDPI AG CY - Basel AN - OPUS4-62698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Mensing, Friedrich A1 - Kruschwitz, Sabine T1 - Estimation of cement content in concrete by spatially resolved laser induced breakdown spectroscopy N2 - The cement content in concrete significantly influences critical properties such as durability, permeability, strength, and workability. Traditional methods for estimating the cement content face limitations. These include the need for comprehensive chemical and solubility knowledge, extensive sample preparation, and their time-consuming and destructive nature. This study investigates the application of laser-induced breakdown spectroscopy (LIBS) as an alternative method. It involves probing concrete samples with high spatial resolution and analyzing the resultant spectra. The methodology is first tested on mesoscale concrete models to assess limitations and inherent errors. Subsequently, the methodology is applied to actual concrete samples with varying cement content and aggregate size distributions. The results demonstrate a promising accuracy, with an average relative error of approximately 8%. This paper offers a comprehensive evaluation of the method's advantages, limitations, and factors influencing its practical applicability in field conditions. KW - LIBS KW - Spectroscopy KW - Cement content KW - Elemental mapping PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-620112 DO - https://doi.org/10.1016/j.cemconres.2024.107714 SN - 1873-3948 VL - 189 SP - 1 EP - 10 PB - Elsevier Ltd. AN - OPUS4-62011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saeidfirozeh, H. A1 - Kubelík, P. A1 - Laitl, V. A1 - Krivkova, A. A1 - Vrabel, J. A1 - Rammelkamp, K. A1 - Schroder, S. A1 - Gornushkin, Igor B. A1 - Kepes, E. A1 - Zabka, J. A1 - Ferus, M. A1 - Porízka, P. A1 - Kaiser, J. T1 - Laser-induced breakdown spectroscopy in space applications: Review and prospects N2 - This review describes the principles and summarizes the challenges of analytical methods based on optical emission spectroscopy (OES) in space applications, with a particular focus on Laser-Induced Breakdown Spectroscopy (LIBS). Over the past decade, LIBS has emerged as a powerful analytical technique for space exploration and In-Situ Resource Utilization (ISRU) of celestial bodies. Its implementation has been suggested for various segments of the Space Resources Value Chain, including prospecting, mining, and beneficiation. Current missions to Mars, including the ChemCam instrument on the Curiosity rover, the SuperCam on the Perseverance rover, and the MarSCoDe on the Zhurong rover, are considered flagship applications of LIBS. Despite neither the Pragyan rover nor the Vikram lander waking from the lunar night, the success of the Chandrayaan-3 mission marks another milestone in the development of LIBS instruments, with further missions, including commercial ones, anticipated. This paper reviews the deployment of LIBS payloads on Mars rovers, upcoming missions prospecting the Moon and asteroids, and LIBS analysis of meteorites. Additionally, it highlights the importance of data processing specific to space applications, emphasizing recent trends in transfer learning. Furthermore, LIBS combined with other spectroscopic techniques (e.g., Raman Spectroscopy, Mass Spectrometry, and Fourier-Transform Infrared Spectroscopy) represents an intriguing platform with comprehensive analytical capabilities. The review concludes by emphasizing the significance of LIBS-based contributions in advancing our understanding of celestial bodies and paving the way for future space exploration endeavors KW - Laser-induced breakdown spectroscopy KW - Mars KW - Moon KW - Asteroids KW - Meteorites KW - Machine learning KW - Transfer learning KW - Raman spectroscopy KW - Mass spectrometry KW - Fourier-transform infrared spectroscopy PY - 2024 DO - https://doi.org/10.1016/j.trac.2024.117991 VL - 181 SP - 1 EP - 22 PB - Elsevier B.V. AN - OPUS4-62142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, Steven A1 - Lippa, Katrice A1 - Shimuzu, Yoshitaka A1 - Lalerle, Beatrice A1 - Saito, Takeshi A1 - Duewer, David A1 - Dai, Xinhua A1 - Davies, Stephen A1 - Ricci, Marina A1 - Baldan, Annarita A1 - Lang, Brian A1 - Sarge, Stefan A1 - Wang, Haifeng A1 - Pratt, Ken A1 - Josephs, Ralf A1 - Mariassy, Mikael A1 - Pfeifer, Dietmar A1 - Warren, John A1 - Bremser, Wolfram A1 - Ellison, Stephen A1 - Toman, Blaza A1 - Nelson, Michael A1 - Huang, Ting A1 - Fajgelj, Ales A1 - Gören, Ahmet A1 - Mackay, Lindsey A1 - Wielgosz, Robert T1 - Methods for the SI-traceable value assignment of the purity of organic compounds (IUPAC Technical Report) N2 - The “purity” of an organic compound typically refers, in practice, to an assignment of the mass fraction content of the primary organic component present in the material. The “purity” value of an organic primary calibrator material is the ultimate source of metrological traceability of any quantitative measurement of the content of that compound in a given matrix. The primary calibrator may consist of a Certified Reference Material (CRM) whose purity has been assigned by the CRM producer or a laboratory may choose to value-assign a material to the extent necessary for their intended application by using appropriately valid methods. This report provides an overview of the approach, performance and applicability of the principal methods used to determine organic purity including mass balance, quantitative NMR, thermal methods and direct-assay techniques. A statistical section reviews best practice for combination of data, value assignment as the upper limit values corresponding to 100 % purity are approached and how to report and propagate the standard uncertainty associated with the assigned values. KW - Calibration hierarchy KW - Certified reference materials KW - Mass balance KW - Measurement uncertainty KW - Organic purity KW - Primary calibrators KW - Primary reference materials KW - qNMR KW - Related-structure impurities KW - Thermal analysis KW - Titrimetry KW - Traceability KW - Uncertainty propagation KW - Volatile organic compounds KW - Water content PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627932 DO - https://doi.org/10.1515/pac-2020-0804 SN - 0033-4545 SN - 1365-3075 VL - 95 IS - 1 SP - 1 EP - 77 PB - de Gruyter CY - Berlin AN - OPUS4-62793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sparber‐Sauer, Monika A1 - Ferrari, Andrea A1 - Kosztyla, Daniel A1 - Ladenstein, Ruth A1 - Cecchetto, Giovanni A1 - Kazanowska, Bernarda A1 - Scarzello, Giovanni A1 - Ljungman, Gustaf A1 - Milano, Giuseppe Maria A1 - Niggli, Felix A1 - Alaggio, Rita A1 - Vokuhl, Christian A1 - Casanova, Michela A1 - Klingebiel, Thomas A1 - Zin, Angelica A1 - Koscielniak, Ewa A1 - Bisogno, Gianni T1 - Long‐term results from the multicentric European randomized phase 3 trial CWS/RMS‐96 for localized high‐risk soft tissue sarcoma in children, adolescents, and young adults N2 - Background: CWS/RMS‐96 was an international multicenter trial with randomization between two therapy arms of the standard four‐drug therapy (vincristine, ifosfamide, adriamycin, dactinomycin [VAIA]) versus an intensified six‐drug regimen (carboplatin, epirubicin, vincristine, dactinomycin, ifosfamide, and etoposide [CEVAIE]) for high‐risk rhabdomyosarcoma (RMS), extraskeletal Ewing sarcoma (EES), and undifferentiated sarcoma (UDS) in children, adolescents, and young adults aiming to improve their survival. Intensified chemotherapy with CEVAIE did not improve outcome. Methods: Patients younger than 21 years with a previously untreated localized HR‐RMS, EES, and UDS were enrolled from Cooperative Weichteilsarkom Studiengruppe (CWS) centers in Germany, Austria, Poland, Switzerland, and from Italian Soft Tissue Sarcoma Committee (STSC) centers. Randomization (1:1) to receive either 9 × 21 days cycles of VAIA or CEVAIE was performed separately in CWS and STSC. Hyperfractionated accelerated radiotherapy (32–44.8 Gy) was added at week 9–12 according to histology and response to chemotherapy. A secondary microscopically complete nonmutilating resection was performed if possible. Primary endpoints were response to chemotherapy, event‐free (EFS) and overall survival (OS). Results: Five hundred fifty‐seven patients (HR‐RMS:n = 416, EES and UDS:n = 141) underwent randomization: VAIA (n = 273) or CEVAIE (n = 284). Radiotherapy was given to 70% of patients in both groups. A secondary resection was performed in 47% and 48% patients, respectively. The 5‐year EFS and OS for the VAIA and CEVAIE treatment arms were 59.8% and 60.8% (p = .89), and 74.2% and 68.3% (p = .16), respectively. No differences in response, toxicity, or second malignancies emerged in the two groups. Conclusion: The use of an intensified regimen failed to show a significant improvement in tumor response and outcome of patients with localized HR‐RMS, EES, and UDS. KW - CEVAIE KW - CWS-96 KW - High-risk soft tissue sarcoma KW - Randomization KW - Rhabdomyosarcoma KW - RMS-96 KW - VAIA PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629373 DO - https://doi.org/10.1002/pbc.29691 SN - 1545-5017 VL - 69 IS - 9 SP - 1 EP - 11 PB - Wiley CY - New York, NY AN - OPUS4-62937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Capozzi, Staci L. A1 - Xia, Chunjie A1 - Shuwal, Matthew A1 - Zaharias Miller, Gillian A1 - Gearhart, Jeff A1 - Bloom, Erica A1 - Gehrenkemper, Lennart A1 - Venier, Marta T1 - From watersheds to dinner plates: Evaluating PFAS exposure through fish consumption in Southeast Michigan N2 - Muscle tissue and organ samples of six different fish species were collected from ten locations in Southeast Michigan’s Huron and Rouge watersheds. Per- and polyfluoroalkyl substances (PFAS) were analyzed in 36 samples comprising filets, liver, gut, and eggs using targeted analysis and the direct total oxidizable precursor (dTOP) assay on a subset of six samples. The median concentrations of the ΣPFAS in filets from the Huron and Rouge watersheds were 13 and 6.3 ng/g wet weight (w.w.), respectively. Perfluorooctane sulfonate (PFOS) was the most detected and abundant compound in fish organs, with the liver having the largest overall burden of PFAS. The highest percent increase in targeted PFAS after the dTOP assay was observed in the Catfish filet (552%) while the smallest increase was in the Catfish liver (32%) accounting for 1.3 and 8.1 nMole F/g dry weight (d.w.), respectively. The positive matrix factorization (PMF) analysis revealed three distinct PFAS sources, of which the one attributed to PFOS explained 73% of the data. Results from this work have important implications for fish consumption in Michigan waterways. Among the filet samples analyzed, the calculated daily consumption limit of total PFOS was exceeded in approximately 82% and 91% of samples for adults and children over the age of seven years old, respectively. KW - Direct total oxidizable precursor (dTOP) assay KW - Huron river watershed KW - Positive matrix factorization (PMF) KW - Rouge river watershed KW - Consumption limit PY - 2023 DO - https://doi.org/10.1016/j.chemosphere.2023.140454 SN - 1879-1298 VL - 345 SP - 1 EP - 9 PB - Elsevier CY - Amsterdam AN - OPUS4-62423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zöllner, Moritz T. A1 - Dariz, Petra A1 - Riedel, Jens A1 - Schmid, Thomas T1 - Dolomite and Mg Calcite as Mineral Thermometers in Mortar Binders. A High Resolution Raman Spectroscopic Study N2 - This paper suggests the use of high‐resolution Raman scattering bands of MgCa carbonates as posteriori thermometer minerals in archaeometric studies. Therefore, the thermal behavior of two dolomite samples and the hydration and carbonation reaction in air of the decomposition products were investigated by Raman microspectroscopy. The increase in the calcination temperature resulted in the formation of – Raman silent MgO and – inert Mg calcite at 700°C–750°C. In contrast, the decarbonation, hydration, and recarbonation of sample material exposed to 750°C–900°C in a muffle furnace led to the appearance of Mg‐free calcite. High spectral resolution Raman spectroscopy enabled a spectral distinction between these two groups due to differences in the band parameters (peak position, bandwidth) of the vibrational (v1, v4, L) modes of calcite. In combination with Raman microspectroscopic mapping, this spectral information represents a new approach for the estimation of burning temperatures of medieval high‐fired gypsum mortars via natural dolomite impurities. Thus, the results of this work highlight the importance and potential of Raman microspectroscopy as a thermometric tool for elucidating the thermal history of anthropogenic fired materials, with potential applications for archaeometry and art technology, as well as for quality controls in the frame of the production of mineral mortar binders and ceramics or bricks, respectively. KW - Mineral thermometry KW - Raman spectroscopy KW - Dolomite KW - High-fired gypsum mortar PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630270 DO - https://doi.org/10.1002/jrs.6810 SN - 1097-4555 SP - 1 EP - 13 PB - Wiley AN - OPUS4-63027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klewe, Tim A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Review of moisture measurements in civil engineering with ground penetrating radar – Applied methods and signal features N2 - When applying Ground Penetrating Radar (GPR) to assess the moisture content of building materials, different medium properties, dimensions, interfaces and other unknown influences may require specific strategies to achieve useful results. Hence, we present an overview of the various approaches to carry out moisture measurements with GPR in civil engineering (CE). We especially focus on the applied Signal features such as time, amplitude and frequency features and discuss their limitations. Since the majority of publications rely on one single feature when applying moisture measurements, we also hope to encourage the consideration of approaches that combine different signal features for further developments. KW - Ground Penetrating Radar KW - Moisture KW - Civil engineering KW - Signal features PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520684 DO - https://doi.org/10.1016/j.conbuildmat.2021.122250 VL - 278 SP - 122250 PB - Elsevier Ltd. AN - OPUS4-52068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Klewe, Tim T1 - Comparison of the Calcium Carbide Method and Darr Drying to Quantify the Amount of Chemically Bound Water in Early Age Concrete N2 - Hydration is the exothermic reaction between anhydrous cement and water, which forms the solid cement matrix of concrete. Being able to evaluate the hydration is of high interest for the use of both conventional and more climate-friendly building materials. The experimental monitoring is based on temperature or moisture measurements. The first needs adiabatic conditions, which can only be achieved in laboratory. The latter is often measured comparing the weight of the material sample before and after oven drying, which is time-consuming. This study investigates the moisture content of two cement-based and two calcium sulphate based mixtures for the first 90 days by using the calcium carbide method and oven drying at 40 °C and 105 °C (Darr method). Thereby, the amount of chemically bound water is determined to derive the degree of hydration. The calcium carbide measurements highly coincide with oven drying at 40 °C. The calcium carbide method is therefore evaluated as a suitable alternative to the time-consuming Darr drying. The prompt results are seen as a remarkable advantage and can be obtained easily in laboratory as well as in the field. KW - Concrete KW - Hydration KW - Material moisture KW - Calcium carbide method KW - Bound water KW - Darr method KW - Oven drying KW - Chemisorption KW - Physisorption PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564519 DO - https://doi.org/10.3390/ma15238422 VL - 15 IS - 23 SP - 1 EP - 16 PB - MDPI AN - OPUS4-56451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -