TY - JOUR A1 - da Silva, D.A. A1 - Greiser, Sebastian A1 - Contro, J. A1 - Medeiros, V.L. A1 - Nery, J.G. A1 - Jäger, Christian T1 - 1H, 29Si and 119Sn double and triple resonance NMR spectroscopy of the small-pore framework sodium stannosilicate Na2SnSi3O9⋅2H2O N2 - The small-pore framework sodium stannosilicate AV-10, chemical composition Na2SnSi3O9⋅2H2O and known crystallographic structure, was synthesized by hydrothermal crystallization. This stannosilicate is built up of a three-dimensional network of corner-shared SiO4 tetrahedra and SnO6 octahedra. The SnO6 sites are linked to six SiO4 tetrahedra (Sn(6Si)) while each of the two crystallographically different SiO4 units are connected to two SnO6 and SiO4 units (Si(2Si,2Sn)). This material was used as model compound for developing a solid-state MAS NMR strategy aimed on the challenges and possibilities for structural studies, particularly considering the short and medium range order to verify the connectivity of SiO4 and SnO6 of such compounds despite the low natural abundances of 4.68% for 29Si and 8.59% for 119Sn nuclei as a real challenge. 29Si{119Sn} and 119Sn{29Si} REDOR (Rotational-Echo Double-Resonance) NMR measurements after 1H cross-polarization (CP) were carried out. The REDOR curves show a significant change after the “normal” quadratic short time evolution from which both (i) the shortest internuclear 29Si – 119Sn distances (and vice versa) and (ii) the number of corner-sharing SiO4 tetrahedra around the SnO6 octahedra (and vice versa) can be obtained. Based on these data, optimized 29Si {119Sn} and 119Sn{29Si} REPT-HMQC (Recoupled Polarization Transfer-Heteronuclear Multiple-Quantum Correlation, again after 1H CP) experiments were implemented, which directly show those heterogroup connectivity as correlation peaks in a 2D spectrum. This information was also obtained using 2D29Si{119Sn}-J-Coupling NMR experiments. Furthermore, 2D29Si INADEQUATE NMR experiments are also feasible, showing the connectivity of SiO4 tetrahedra. The combination of REDOR, REPT-HMQC, J-Coupling and INADEQUATE experiments yielded a complete analysis of the short and medium range structure of this microporous stannosilicate, in agreement with the previously published structure obtained Ab Initio from powder X-Ray diffraction data (XRD). KW - Stannosilicates KW - REDOR KW - REPT-HMQC KW - INADEQUATE PY - 2020 DO - https://doi.org/10.1016/j.ssnmr.2020.101661 SN - 0926-2040 VL - 107 SP - 101661 PB - Elsevier Inc. AN - OPUS4-50710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - da Silva, Luiza Helena Bueno A1 - Goes, Aryel C. A1 - Rodrigues, Andre A1 - Fourcassié, Vincent A1 - McMahon, Dino Peter A1 - Haifig, Ives T1 - Social immune response reflects infection progression in a soldierless termite N2 - Social interactions represent a double-edged sword. On one hand, sociality can facilitate sanitary collective behaviours; on the other hand, it creates opportunities for pathogen transmission. In termites, sanitary behaviours can entail a rescuing strategy at early stages of infection, followed by the elimination at later stages. We explored whether the neotropical soldierless species Anoplotermes pacificus employs a progressive approach towards infected nestmates, with different behavioural displays depending on the infection stage. We infected A. pacificus workers with the fungus Metarhizium anisopliae and incubated them for 2, 12, 15 and 20 h, corresponding to infection progression and, therefore, severity. Infected termites were placed with naïve nestmates and their behaviours were recorded for 3 h. Fungus-infected termites triggered up to fourfold higher levels of sanitary behaviour than in non-infected termites. Antennation behaviour decreased during the observation period, whereas sanitary behaviour, which we defined as directed behaviour towards the focal termite involving mouthparts, increased in frequency as incubation duration increased. Sanitary behaviour therefore appears to be a strategy for colony disinfection, which varies in intensity according to infection status, ultimately resulting in the immobilisation of infected individuals at later stages of infection. Alarm responses were also up to three times more frequent in treatment than in control groups and did not vary with incubation duration. A. pacificus workers therefore identify, communicate and respond to pathogen-treated individuals in a progressive manner, indicating that collective responses in this species are also significantly shaped by the stage of infection. By progressively modulating their social immune responses, termites may be able to optimize resource allocation within the colony by balancing the risk of individual infection versus protection of the group. KW - Anoplotermes pacificus KW - Isoptera KW - Infection KW - Metarhizium KW - Social immunity PY - 2024 DO - https://doi.org/10.1007/s00265-024-03556-2 VL - 79 IS - 1 SP - 1 PB - Springer Science and Business Media LLC AN - OPUS4-62397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Bettencourt da Silva, R. A1 - Bulska, E. A1 - Godlewska-Zytkiewicz, B. A1 - Hedrich, Martina A1 - Majcen, N. A1 - Magnusson, B. A1 - Marincic, S. A1 - Papadakis, I. A1 - Patriarca, M. A1 - Vassileva, E. A1 - Taylor, P. ED - Majcen, N. ED - Gegevicius, V. T1 - Measurement uncertainty and statistics N2 - TrainMiC® is a European programme for lifelong learning on how to interpret the metrological requirements in chemistry. It is operational across many parts of Europe via national teams. These teams use shareware pedagogic tools which have been harmonised at European level through the joint effort of many experts across Europe working as an editorial board. The material has been translated into 14 different languages. This report includes four TrainMiC® presentations: 1. Uncertainty of measurement — Part I Principles; 2. Uncertainty of measurement — Part II Approaches to evaluation; 3. Statistics for analytical chemistry — Part I; and 4. Statistics for analytical chemistry — Part II KW - Chemistry KW - Statistical method KW - Scientific research KW - Materials technology KW - Research report KW - Measurement uncertainty KW - Statistics PY - 2013 SN - 978-92-79-23070-7 DO - https://doi.org/10.2787/5825 SN - 1018-5593 IS - JRC 68476 SP - Chapter 1-4, 19-230 AN - OPUS4-32534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miccoli, Lorenzo A1 - Müller, U. A1 - Silva, B. A1 - Da Porto, F. A1 - Hracov, S. A1 - Pospisil, S. A1 - Adami, C.-E. A1 - Vintzileou, E. A1 - Vasconcelos, G. A1 - Poletti, E. ED - Jasienko, J. T1 - Overview of different strengthening techniques applied on walls used in historical structures T2 - SAHC 2012 - 8th International conference on structural analysis of historical constructions CY - Wroclaw, Poland DA - 2012-10-15 KW - Stone masonry KW - Brick masonry KW - Earthen materials KW - Half timbered walls KW - Grouting PY - 2012 SN - 978-83-7125-216-7 SN - 0860-2395 VL - 3 SP - 2870 EP - 2878 PB - DWE CY - Wroclaw, Poland AN - OPUS4-27275 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 - JOUR A1 - da Silva, T. R. A1 - Matos, P. R. de A1 - Durlo Tambara, Luís Urbano A1 - Marvila, M. T. A1 - de Azevedo, A. R. G. T1 - A review on the performance of açaí fiber in cementitious composites: Characteristics and application challenges N2 - This paper aimed to perform an exploratory literature review, focusing on the aspects of hydration and rheological properties of cementitious composites with açaí fibers. The use of natural fibers as a reinforcement in cementitious matrices has been widely studied, and açaí fiber is a promising option due to its unique characteristics. However, there is still a lack of knowledge regarding the correlation between fiber parameters and the technological properties of composites, which limits the development of new applications, such as 3D printing. The review provided an overview of the main characteristics of açaí fibers and the parameters for their application in cementitious matrices. Alkali treatment with 5% NaOH solution for 1 h shows increased mechanical and physical properties in açaí fibers. Despite the potential advantages of these composites, they pose challenges due to the different fiber surface treatment and interfacial transitions and the processing conditions of the fibers. Although small addition of açaí fibers slightly decreases the cement hydration process, keeping the cross-compatibility index high (>95). To overcome these challenges, it is necessary to evaluate the rheological behavior of cementitious materials with açaí fibers, which has not been reported in the literature. By doing so, it will be possible to optimize the processing conditions and develop new applications, such as additive manufacturing, which has never been explored with açaí fibers. KW - Natural fibers KW - Açaí fiber KW - Portland cement KW - Alternative materials PY - 2023 DO - https://doi.org/10.1016/j.jobe.2023.106481 SN - 2352-7102 VL - 71 IS - 106481 SP - 1 EP - 21 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-57326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. D. A1 - Choteau, T. A1 - Martos, G. A1 - Wielgosz, R. A1 - Sarzuri, Y. A. A1 - Mendoza, E. A1 - do Rego, E. C. P. A1 - Violante, F. G. M. A1 - da Silva Souza, W. A1 - de Carvalho, L. J. A1 - Fernandes, J. L. N. A1 - Bates, J. A1 - Rajotte, I. A1 - Melanson, J. E. A1 - Li, H. A1 - Guo, Z. A1 - Su, F. A1 - Wang, S. A1 - Huang, T. A1 - Lalerle, B. A1 - Gantois, F. A1 - Piechotta, Christian A1 - Philipp, Rosemarie A1 - Kaminski, Katja A1 - Klyk-Seitz, Urzsula-Anna A1 - Giannikopoulou, P. A1 - Skotidaki, E. A1 - Kakoulides, E. A1 - Pui-Kwan, C. A1 - Kuroe, M. A1 - Itoh, N. A1 - Calderón, M. A. A. A1 - Contreras, L. R. A1 - Osuna, M. A. A1 - Alrashed, M. A1 - Ting, L. A1 - Mei, G. E. A1 - Juan, W. A1 - Sze, C. P. A1 - Lin, T. T. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Ahn, S. A1 - Chaiphet, T. A1 - Sudsiri, N. A1 - Bellazreg, W. A1 - Bilsel, M. A1 - Colombo, G. T1 - Key comparison CCQM-K78.b - non-polar analytes in organic solvent: methoxychlor and trifluralin in acetonitrile N2 - The CCQM-K78.b key comparison was coordinated by the Bureau International des Poids et Mesures (BIPM) on behalf of the CCQM Organic Analysis Working Group (OAWG) of the 'Comité Consultatif pour la Quantité de Matière' (CCQM), for National Measurement Institutes (NMIs) and Designated Institutes (DIs) providing measurement services in organic analysis under the 'Comité International des Poids et Mesures' (CIPM) Mutual Recognition Arrangement (MRA). This key comparison was conducted as a 'Track A' comparison within the OAWG's 10-year strategic plan. The goal of CCQM-K78.b was to underpin capabilities for the value assignment of calibration solutions containing low polarity/non-polar organic analytes in organic solvents. The selected model system consisted of a two-component pesticide solution in acetonitrile, comprising methoxychlor and trifluralin. Participants were tasked with assigning the mass fractions, in units of μg/g, of methoxychlor and trifluralin in acetonitrile solution. The mass fraction levels and analytical challenges of the selected analytes were representative of those encountered for calibration solutions of non-polar organic analytes. Participation in CCQM-K78.b allowed for the benchmarking of capabilities for assigning the mass fraction of non-polar organic compounds (pKow < -2) in solution, at mass fractions above 5 μg/g, in an organic solvent. Additionally, the comparison assessed the capabilities for the quantitative assignment of thermally labile compounds. Participants were provided by the BIPM with ampoules containing methoxychlor and trifluralin in acetonitrile. Each participant reported the mass fraction content of each analyte in μg/g. All participants ensured the metrological traceability of their results through the use of a Primary Reference Material (PRM), which was used to prepare a primary calibrator solution for each analyte using a gravimetric procedure. The twenty participating institutes primarily used analysis procedures based on GC-MS, -IDMS, -MS/MS, -ECD, and -FID, with some participants also using LC-UV for the value assignment. The analysis of methoxychlor and trifluralin in acetonitrile solution presented several challenges, including the thermal stability of the analytes under selected analytical techniques, control of solvent volatility, and considerable variation in some results using MS-based quantification methods. The mass fraction assignments for methoxychlor and trifluralin, consistent with the key comparison reference values (KCRVs), were achieved with associated relative standard uncertainties of (0.38 - 2.9) % for methoxychlor and (0.35 - 2.5) % for trifluralin. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - Methoxychlor KW - Trifluralin KW - CCQM KW - Key comparison PY - 2025 DO - https://doi.org/10.1088/0026-1394/62/1A/08010 SN - 0026-1394 VL - 62 IS - 1A SP - 1 EP - 37 PB - IOP Publishing AN - OPUS4-64691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darvishi Kamachali, Reza A1 - da Silva, A. A1 - McEniry, E. A1 - Gault, B. A1 - Neugebauer, J. A1 - Raabe, D. T1 - Segregation-assisted spinodal and transient spinodal phase separation at grain boundaries N2 - Segregation to grain boundaries affects their cohesion, corrosion, and embrittlement and plays a critical role in heterogeneous nucleation. In order to quantitatively study segregation and low-dimensional phase separation at grain boundaries, here, we apply a density-based phase-field model. The current model describes the grain-boundary thermodynamic properties based on available bulk thermodynamic data, while the grain-boundary-density profile is obtained using atomistic simulations. To benchmark the performance of the model, Mn grain-boundary segregation in the Fe–Mn system is studied. 3D simulation results are compared against atom probe tomography measurements conducted for three alloy compositions. We show that a continuous increase in the alloy composition results in a discontinuous jump in the segregation isotherm. The jump corresponds to a spinodal Phase separation at grain boundary. For alloy compositions above the jump, we reveal an interfacial transient spinodal phase separation. The transient spinodal phenomenon opens opportunities for knowledge-based microstructure design through the chemical manipulation of grain boundaries. The proposed density-based model provides a powerful tool to study thermodynamics and kinetics of segregation and phase changes at grain boundaries. KW - Grain Boundary Spinodal KW - Densty-based Thermodynamics KW - Microstrucrue Design PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519497 DO - https://doi.org/10.1038/s41524-020-00456-7 VL - 6 IS - 1 SP - 191 PB - Nature AN - OPUS4-51949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mesquita Silva da Veiga, Marcia T1 - Ultrasonic-assisted leaching of Li and Co from black mass using deep eutectic solvent N2 - The recovery of critical metals from spent lithium-ion batteries is a key strategy for sustainable resource management and the circular economy. Conventional hydrometallurgical processes typically rely on strong mineral acids and elevated temperatures, which, although effective, generate hazardous waste and demand high energy inputs. As a greener alternative, deep eutectic solvents (DES) combine low toxicity, non-volatility, simple synthesis, and tunable physicochemical properties, making them promising media for selective metal recovery1-2. Here, we report for the first time the use of ultrasound (US) to assist the leaching of Li and Co from LiCoO₂ black mass employing a deep eutectic solvent based on choline chloride and formic acid (ChCl:HCOOH, 1:2 molar ratio). The DES was synthesized at 90 °C for 3 h under stirring (300 rpm) and was characterized in terms of its molecular structure and formation by 1H-NMR and FT-IR, as well as by its viscosity and density. For each experiment, ~0.100 g of LiCoO2 was treated with 5 g of DES-FA in an ultrasonic bath (35 kHz, 60 °C) for different irradiation times (30–120 min), followed by three sequential extractions. All measurements were performed by ICP OES. Lithium solubilization reached ~80% at 90 min, while cobalt extraction was stabilizing at ~79% after 120 min. The enhanced performance under US is attributed to sonochemical effects that promote cavitation and microjets, leading to the disruption of particle agglomerates, the thinning of diffusion layers, and the generation of highly reactive local environments. These processes accelerate deintercalation and mass transfer within the solid–liquid interface. Combined with the mild acidity of DES-FA, which enables simultaneous leaching of both metals while favoring faster kinetics for Li, ultrasound provided a synergistic effect that enhanced the overall process and preserved the distinct extraction profiles of Li and Co. The extraction behavior of the two metals can be explained by their different speciation in the DES-FA medium. Cobalt is likely reduced from Co(III) to Co(II) by formic acid and stabilized through the formation of chloro-complexes such as [CoCl4]2- with chloride anions from ChCl, favoring its solubilization. In contrast, lithium does not form stable complexes with chloride under these conditions. It is primarily extracted as a solvated cation, stabilized by the extensive hydrogen-bond network of the DES. This difference accounts for the faster leaching kinetics observed for Li compared to Co. Selective recovery was achieved by pHcontrolled precipitation, with cobalt oxalate at pH 4-5 and lithium carbonate at pH 10. The Eco-Scale score of 85 confirmed the greenness of the method. This pioneering approach highlights the potential of coupling DES chemistry with ultrasound. Together, they represent a sustainable and efficient route for recovering critical metals from battery waste. T2 - 17th Rio Symposium on Atomic Spectrometry (17th RSAS) CY - São Pedro City, Brazil DA - 09.11.2025 KW - Black mass KW - deep eutectic solvent KW - Lithium KW - Cobalt KW - Lithium-ion battery recycling KW - Ultrasound-assisted extraction KW - Lithium and cobalt recovery KW - Green hydrometallurgy PY - 2025 AN - OPUS4-64956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arai, Marylyn Setsuko A1 - Machado, Thales Rafael A1 - da Silva, Beatriz Giacomelli Rodrigues A1 - Vilela, Raquel Riciati do Couto A1 - de Camargo, Andrea Simone Stucchi A1 - Zucolotto, Valtencir T1 - Biomimetic Upconverting Nanoplatforms for Glioblastoma Bioimaging and Targeted Therapy N2 - Infectious bacterial diseases, intensified by antibiotic resistance, cause millions of deaths annually and pose risks beyond human health, including water and food contamination. Current diagnostics are often slow, require complex equipment, and lack specificity, highlighting the need for rapid and reliable detection methods. To address this, we developed a luminescent sensor based on NaYF4 upconverting nanoparticles (UCNPs) doped with Er3+ or Tm3+, coated with COOH-PEG4-COOH, and functionalized with vancomycin (Van) or polymyxin-B (Poly) to selectively target Gram-positive and Gram-negative bacteria, respectively. Gold nanoparticles (AuNPs) served as quenchers, enabling a ratiometric “turn-on” mechanism: upon bacterial binding, the UCNP emission, initially quenched by AuNPs, was partially restored. This allowed differentiation through changes in the green/red (G/R) ratio for Er-UCNP@PEG4-Van and the blue/red (B/R) ratio for Tm-UCNP@PEG4-Poly. The sensor distinguished between Gram-positive and Gram-negative bacteria over a wide concentration range (0.05 to 5 × 105 CFU/mL) and showed high correlation with actual bacterial counts (r = 0.99 for S. aureus, r = 0.91 for E. coli). This platform is a potential fast, selective, and reliable tool for bacterial detection in clinical and environmental settings. KW - Glioblastoma KW - Homotypic targeting KW - Cell membrane coating KW - Upconverting nanoparticles KW - Temozolamide KW - Near infrared bioimaging KW - Drug delivery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652808 DO - https://doi.org/10.1021/acsanm.5c04567 SN - 2574-0970 VL - 10 IS - 39 SP - 1 EP - 13 PB - American Chemical Society (ACS) AN - OPUS4-65280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -