TY - JOUR A1 - Capitain, C. A1 - Schüßler, M. A1 - Bugsel, B. A1 - Zweigle, J. A1 - Vogel, Christian A1 - Leube, Peter A1 - Zwiener, C. T1 - Implementation of matrix-matched semiquantification of PFAS in AFFF-contaminated soil N2 - This study presents a novel semiquantification approach for nontarget screening (NTS), combining matrix-matched calibration and ionization class-specific average calibration curves (ACCs) to address the lack of analytical reference standards for most per- and polyfluoroalkyl substances (PFAS). Ionization class-specific ACCs for carboxylic and sulfonic acids, sulfonamides, and cationic PFAS result in high accuracy, with median absolute accuracy quotients below 2.27×. The approach was applied to soil impacted by aqueous film-forming foam (AFFF) contamination. A total of 96 tentatively identified PFAS were semiquantified in addition to 28 quantified compounds based on available standards. Semiquantified concentrations exceeded those of target analytes, demonstrating the critical role of this method in capturing broader PFAS contamination. In this case, validation against extractable organofluorine (EOF) showed a 102% closed mass balance. The innovative approach not only enables comprehensive PFAS contamination assessment in complex matrices but also expands the scope of the NTS for environmental monitoring, remediation, and risk assessment of AFFF-contaminated sites. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Contaminated soil KW - Non-targeted analysis KW - Combustion ion chromatography PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629445 DO - https://doi.org/10.1021/acs.est.4c14255 SN - 1520-5851 VL - 59 IS - 14 SP - 7338 EP - 7347 PB - American Chemical Society (ACS) CY - Columbus, Ohio AN - OPUS4-62944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - McGonigle, Rebecca A1 - Glasgow, Jodie A1 - Houston, Catriona A1 - Cameron, Iain A1 - Homann, Christian A1 - Black, Dominic J. A1 - Pal, Robert A1 - MacKenzie, Lewis E. ED - MacKenzie, Lewis E. T1 - Autoclave reactor synthesis of upconversion nanoparticles, unreported variables, and safety considerations N2 - Autoclave reactors are widely used across chemical and biological sciences, including for the synthesis of upconversion nanoparticles (UCNPs) and other nanomaterials. Yet, the details of how autoclave reactors are used in such synthesis are rarely reported in the literature, leaving several key synthesis variables widely unreported and thereby hampering experimental reproducibility. In this perspective, we discuss the safety considerations of autoclave reactors and note that autoclaves should only be used if they are (a) purchased from reputable suppliers/manufacturers and (b) have been certified compliant with relevant safety standards. Ultimately, using unsuitable autoclave equipment can pose a severe physical hazard and may breach legal safety requirements. In addition, we highlight several parameters in autoclave synthesis that should be reported as standard to maximise the reproducibility of autoclave synthesis experiments across materials and chemistry research. We encourage users of autoclave synthesis vessels to: (1) adopt high-safety autoclaves and (2) report the many experimental variables involved to enhance experimental reproducibility. KW - Reference material KW - Nano KW - Particle KW - Shell KW - Fluorescence KW - Lifetime KW - Decay kinetics KW - Synthesis KW - Quality assurance KW - Method KW - Energy transfer KW - Upconversion KW - Autoclave synthesis KW - Data comparability PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625672 DO - https://doi.org/10.1038/s42004-025-01415-3 VL - 8 IS - 1 SP - 1 EP - 7 PB - Springer Science and Business Media LLC AN - OPUS4-62567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poka, Konstantin A1 - Ali, Sozol A1 - Saeed, Waleed A1 - Merz, Benjamin A1 - Epperlein, Martin A1 - Hilgenberg, Kai T1 - Quality assurance via a cyber physical system of a PBF-LB/M machine N2 - Powder Bed Fusion with Laser Beam of Metals (PBF-LB/M) faces challenges in reproducibility and quality assurance, even for widely applied alloys like AlSi10Mg. This work introduces a digital provenance framework for PBF-LB/M, showcased through the EOS M 300–4 multi-laser machine. An Extract, Transform, Load (ETL) pipeline autonomously captures machine data, including scan vectors as well as process signals, and organizes them into a Digital Shadow (DS). The DS is further extended by external data sources, such as Melt Pool Monitoring (MPM), to enable comprehensive analysis and root cause identification. This approach ensures continuous data representation and facilitates the development of new quality metrics. Moreover, the framework enhances quality assurance and traceability, supports compliance with industry standards, and improves productivity. It also enables more precise cost calculations and predictive maintenance. By addressing these challenges, the framework is essential for advancing PBF-LB/M in industrial applications, achieving greater consistency and scalability in production. KW - PBF-LB/M KW - Data driven quality assurance KW - Data engineering KW - Digital shadow PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625187 DO - https://doi.org/10.1007/s40964-025-00978-w SN - 2363-9520 VL - 10 IS - 3 SP - 1771 EP - 1783 PB - Springer Science and Business Media LLC AN - OPUS4-62518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schackmann, Oliver A1 - Márquez Reyes, Octavio A. A1 - Memmolo, Vittorio A1 - Lozano, Daniel A1 - Prager, Jens A1 - Moll, Jochen A1 - Kraemer, Peter T1 - Machine learning strategies with ensemble voting for ultrasonic damage detection in composite structures under varying temperature or load conditions N2 - In recent years, the development of machine learning (ML) techniques has led to significant progress in the field of structural health monitoring with ultrasonic-guided waves. However, a number of challenges still need to be resolved for reliable operation in realistic settings. In this work, we consider the complex problem of experimental damage detection under varying temperature or load conditions where damage locations are not included in the training set. The ML techniques proposed here include supervised and unsupervised methods originally developed for image and time series classification combined with ensemble voting. A performance demonstration of the ML techniques is presented using benchmark datasets from the open-guided waves platform. The unsupervised approach is then applied to a new dataset from an experimental campaign carried out on a composite over-wrapped pressure vessel used for hydrogen storage with real defects. Results show that ensemble voting enables the effective combination of the predictions of multiple transducer pairs, even with a limited number of strong individual classifiers. When applied to unsupervised learning, this returns high accuracy also when real damage over the structure is considered. KW - Structural-Health-Monitoring KW - Ultrasonic guided waves PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631571 DO - https://doi.org/10.1177/14759217251333066 SN - 1741-3168 SP - 1 EP - 19 PB - Sage Publications AN - OPUS4-63157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hendricks, A. A1 - Phillips, T. K. A1 - Engl, T. A1 - Plarre, Rudy A1 - Martinson, V. G. T1 - The bacterial microbiome in spider beetles and deathwatch beetles N2 - The beetle family Ptinidae contains a number of economically important pests, such as the cigarette beetle Lasioderma serricorne, the drugstore beetle Stegobium paniceum, and the diverse spider beetles. Many of these species are stored product pests, which target a diverse range of food sources, from dried tobacco to books made with organic materials. Despite the threat that the 2,200 species of Ptinidae beetles pose, fewer than 50 have been surveyed for microbial symbionts, and only a handful have been screened using contemporary genomic methods. In this study, we screen 116 individual specimens that cover most subfamilies of Ptinidae, with outgroup beetles from closely related families Dermestidae, Endecatomidae, and Bostrichidae. We used 16S ribosomal RNA gene amplicon data to characterize the bacterial microbiomes of these specimens. The majority of these species had never been screened for microbes. We found that, unlike in their sister family, Bostrichidae, that has two mutualistic bacteria seen in most species, there are no consistent bacterial members of ptinid microbiomes. For specimens which had Wolbachia infections, we did additional screening using multilocus sequence typing and showed that our populations have different strains of Wolbachia than noted in previous publications. KW - Sodalis KW - Ptinidae KW - Anobiidae KW - Bostrichidae KW - Dermestidae KW - Bostrichoidea KW - Wolbachia PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631564 DO - https://doi.org/10.1128/spectrum.01981-24 SN - 2165-0497 VL - 13 IS - 5 SP - 1 EP - 14 AN - OPUS4-63156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Amano, Kofi Owusu Ansah A1 - Tschirschwitz, Rico A1 - Gimadieva, Elena A1 - Köhler, Florian A1 - Krause, Ulrich T1 - Thermal runaway and explosibility of the gas release from 18650 sodium-ion cells of NFM chemistry N2 - The present study investigates the thermal runaway behaviour and explosibility of the gas mixture released from sodium-ion batteries (SIBs). A total of 30 tests comprising two test series were performed using 18650 SIBs with a NaNi1/3Fe1/3Mn1/3O2 (NFM) chemistry. The cells of SOC level = 0 %, 25 %, 50 %, 75 % and 100 % were subjected to thermal abuse inside a 10 L pressurized reaction vessel. In test series 1, the tests were performed in an air atmosphere. In test series 2, an inert atmosphere was used. First, the total amount of gas released from the SIBs was calculated based on the temperature and pressure measured in the reaction vessel. Subsequently, a gas composition analysis was performed using a Fourier-transformed infrared (FTIR) spectrometer. This study revealed that the thermal runaway in SIBs could be categorized into four phases. At the onset of thermal runaway, the thermal runaway-induced explosion of the cells resulted in a rate of temperature rise ranging from 2 K/s to 70 K/s. The investigation further revealed a peak reaction temperature of 415 ◦C and a maximum pressure of 4 bar could be reached at thermal runaway in the 10 L vessel. The gas release of up to 5 ± 0.3 L (4 ± 0.2 L/Ah, 1.3 ± 0.1 L/Wh) from test series 1 and 2.4 ± 0.2 L (2 ± 0.1 L/Ah, 0.53 ± 0.04 L/Wh) from test series 2 showed a dependence on SOC and failure environment used. By applying Le Chatelier's mixing rule, the measured gas release from the air atmosphere showed a calculated lower explosion limit and upper explosion limit values of 4.8 % and 24 % in volume fraction, respectively. KW - Sodium-ion battery KW - Thermal runaway KW - Gas release KW - Gas explosion KW - Explosion limit PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631782 DO - https://doi.org/10.1016/j.est.2025.116614 SN - 2352-152X VL - 122 SP - 1 EP - 16 PB - Elsevier Ltd. AN - OPUS4-63178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jafari, Abbas A1 - Vlachas, K. A1 - Chatzi, E. A1 - Unger, Jörg F. T1 - A Bayesian framework for constitutive model identification via use of full field measurements, with application to heterogeneous materials N2 - In this paper, we present a Bayesian framework for the identification of the parameters of nonlinear constitutive material laws using full-field displacement measurements. The concept of force-based Finite Element Model Updating (FEMU-F) is employed, which relies on the availability of measurable quantities such as displacements and external forces. The proposed approach particularly unfolds the advantage of FEMU-F, as opposed to the conventional FEMU, by directly incorporating information from full-field measured displacements into the model. This feature is well-suited for heterogeneous materials with softening, where the localization zone depends on the random microstructure. Besides, to account for uncertainties in the measured displacements, we treat displacements as additional unknown variables to be identified, alongside the constitutive parameters. A variational Bayesian scheme is then employed to identify these unknowns via approximate posteriors under the assumption of multivariate normal distributions. An optimization problem is then formulated and solved iteratively, aiming to minimize the discrepancy between true and approximate posteriors. The benefit of the proposed approach lies in the stochastic nature of the formulation, which allows to tackle uncertainties related to model parameters and measurement noise. We verify the efficacy of our proposed framework on two simulated examples using gradient damage model with a path-dependent nonlinear constitutive law. Based on a nonlocal equivalent strain norm, this constitutive model can simulate a localized damage zone representing softening and cracking. The first example illustrates an application of the FEMU-F approach to cracked structures including sensitivity studies related to measurement noise and parameters of the prior distributions. In this example, the variational Bayesian solver demonstrates a sizable advantage in terms of computational efficiency compared to a traditional least-square optimizer. The second example demonstrates a sub-domain analysis to tackle challenges associated with limited domain knowledge such as uncertain boundary conditions. KW - Constitutive model identification KW - Full-field measurements KW - Variational Bayes KW - Force-based finite element model updating KW - FEMU-F PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615476 DO - https://doi.org/10.1016/j.cma.2024.117489 SN - 1879-2138 VL - 433 IS - Part A SP - 1 EP - 32 PB - Elsevier B.V. AN - OPUS4-61547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, A. A1 - Simkin, Roman T1 - Identifying the initial corrosion fatigue failure based on dropping electrochemical potential N2 - The corrosion fatigue of duplex stainless-steel X2CrNiMoN22-5-3 can be determined by purely alternating axial cyclic load to failure using hour-glass shaped specimens. The experimental setup comprises a corrosion chamber allowing for the circulation of an aquifer electrolyte heated to 369 K simulating a carbon capture and storage as well as geothermal power plant environment. During engineering of a carbon storage site or geothermal power plant, it may be crucial to determine the failure onset of a component beforehand. Therefore, an algorithm with 93.3% reliability was established based on splitting the measured potential values into ten time series with a capacity of ten values. The failure of corrosion fatigue specimens in a geothermal environment correlates to the drop of the curves of the electrochemical potential which is measured simultaneously within the corrosion chamber. Crack initiation was, therefore, successfully derived from the electrochemical potential. KW - Corrosion fatigue KW - Surface corrosion KW - CO2 KW - Crack initiation KW - Geothermal energy production PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629310 DO - https://doi.org/10.3390/app15010403 SN - 2076-3417 VL - 15 IS - 1 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-62931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kumar, Sumit A1 - Swaminathan, Srinivasan A1 - Hesse, Rene A1 - Goldbeck, Hennig A1 - Ding, Wenjin A1 - Bonk, Alexander A1 - Bauer, Thomas T1 - Understanding the effect of oxide ions on Solar Salt chemistry and corrosion mechanism of 316L stainless steel at 600 °C N2 - Solar Salt (60 wt% NaNO3, 40 wt% KNO3), used in Concentrated Solar Power (CSP) Thermal Energy Storage (TES) technology, can decompose into various products at elevated temperatures, with oxide ions being one of the known corrosive byproducts. The study mimics Solar Salt aging by intentionally adding sodium peroxide (Na2O2) and sodium oxide (Na2O) at concentrations of 0.005–0.33 wt% to investigate their role in the corrosion of austenitic stainless steel at 600 °C in typical operating conditions. Salt chemistry (nitrite, nitrate, oxide ions, and metal cations) was analyzed every 24 h, and steel corrosion after 168 h was assessed by weight change, corrosion rate, phase analysis, and cross-sectional morphology. Results reveal that at or above 0.135 wt% added Na2O2/Na2O leads to a quasi-steady-state equilibrium of oxide ions in the salt. Interestingly, at these concentrations, the presence of steel further decreases oxide ion concentration. Furthermore, above 0.135 wt%, the corrosion rate increases significantly, along with increased spallation, porosity and disintegration of the corrosion layer, forming a non-protective layer. This study highlights the critical role of oxide ions in the corrosion process. KW - Solar Salt KW - High temperature corrosion KW - Thermal Energy Storage KW - Alkali oxides KW - Austenitic stainless steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628463 DO - https://doi.org/10.1016/j.corsci.2025.112849 SN - 1879-0496 VL - 249 SP - 1 EP - 17 PB - Elsevier Ltd. AN - OPUS4-62846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - John, Elisabeth A1 - Jakob, Cordula A1 - Pott, Ursula A1 - Sando, Mona T1 - Repeatability and reproducibility challenges of isothermal heat flow calorimetry with in situ mixing N2 - Isothermal heat flow calorimetry evaluates heat development during binder reactions. It distinguishes between in situ calorimetry, where mixing occurs within the device, and ex situ calorimetry, involving externally mixed samples. Despite ex situ calorimetry being a standard method in binder research, in situ calorimetry is underutilized. This paper aims to promote its adoption by summarizing challenges related to repeatability and reproducibility and offering solutions. The initial section addresses repeatability issues caused by preventable errors, providing a structured guide for experimental design. It was found that water leakage had minimal impact, and sample size is crucial for data robustness. The second section examines operational challenges, revealing that frictional heating, affecting recorded heat, can be minimized with an optimized mixing protocol. The final part highlights that significant errors in measured data stem from signal delay and heat loss, offering methods to correct these issues for improved reproducibility in in situ calorimetric experiments. KW - In situ calorimetry PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628431 DO - https://doi.org/10.1016/j.cemconres.2025.107872 SN - 1873-3948 VL - 194 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-62843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -