TY - JOUR
A1 - El-Dahshan, O.
A1 - Deniaud, A.
A1 - Ling, W. L.
A1 - Wegner, Karl David
A1 - Proux, O.
A1 - Veronesi, G.
A1 - Reiss, P.
T1 - Hydrothermal microwave synthesis of water soluble NIR-II emitting Ag2S quantum dots
N2 - Hydrothermal-based synthetic methods of quantum dots allow for the exploration of reaction parameters normally inaccessible to typical aqueous-based batch reactions, such as elevated reaction temperatures (>100 °C) and reaction pressures above atmospheric pressure. Coupled with microwave heating, new instantaneously bio-compatible quantum dots (QDs) with enhanced opitcal properties can be yielded. As of today, aqueous-based synthetic methods often lag behind their organic analogues in terms of the photophysical properties of the QDs obtained and the ease of modulation of both the emission wavelength and crystallite size. Using a novel microwave-assisted hydrothermal approach, the synthesis of silver sulphide (Ag2S) QDs exhibiting NIR emission spanning the biological transparency windows via modulation of the reaction parameters has been developed. The intrinsic link between their optical and structural properties is explored via laboratory and synchrotron-based structural analysis techniques. Their toxicity towards a hepatic cell line was assessed, and related back to their structure and size. Overall this work aims to not only further develop the repertoire of synthetic methods for the synthesis of Ag2S QDs, but also paves the way for the development of safer QDs suitable for future clinical applications.
KW - Quantum dots
KW - Microwave synthesis
KW - Quality assurance
KW - NIR-II emission
KW - PL quantum yield
KW - Ag2S
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634825
DO - https://doi.org/10.1039/d5nr00052a
SN - 2040-3372
VL - 17
IS - 24
SP - 14637
EP - 14646
PB - RSC
AN - OPUS4-63482
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Yu, Jialu
A1 - Oelze, Marcus
A1 - Schannor, Mathias
A1 - Nordstad, Simon
A1 - Vogl, Jochen
T1 - New Potential Haematite and Magnetite Reference Materials for Iron Isotope Measurements by Solution Nebulisation MC ‐ ICP ‐ MS and by In Situ ns ‐ LA ‐ MC ‐ ICP ‐ MS
N2 - Iron isotope ratios of haematite (Fe2O3) and magnetite (Fe3O4) provide insights into geochemical, environmental and planetary processes. In most studies, Fe isotope measurements are commonly performed using solution nebulisation multi-collector inductively coupled plasma-mass spectrometry (SN-MC-ICP-MS). Nanosecond laser ablation multi-collector inductively coupled plasma-mass spectrometry (ns-LA-MC-ICP-MS) requires minimal sample preparation, and provides spatially resolved variation of iron isotopes at micro-scale. However, homogeneous and matrix-matched haematite/magnetite reference materials are lacking for precise in situ isotopic measurement. The iron isotope ratios of two potential reference materials resembling natural haematite (HMIE-NP-B01) and natural magnetite (MAKP-NP-B01) were characterised. Size fractions between 5–63 μm of the powdered Fe oxides were milled to nanoparticles, freeze-dried, homogenised, and pressed into pellets. The materials were then evaluated using SN-MC-ICP-MS and LA-MC-ICP-MS. Sample powders of the two materials were measured by SN-MC-ICPMS after sample digestion and column separation and pressed pellets were analysed directly via ns-LA-MC-ICP-MS. In both cases iron isotope delta values are reported relative to the certified reference material IRMM-014, used as the bracketing standard (calibrator). The solution measurements yielded δ56Fe values of -0.25 ± 0.08‰ (N = 13, 2s) for HMIE-NP-B01, and -0.05 ± 0.09‰ (N = 12, 2s) for MAKP-NP-B01, considered as the preferred Fe isotope delta values. In situ isotopic analysis via ns-LA-MC-ICP-MS yielded δ56Fe values of -0.28 ± 0.28‰ (N = 19, 2s) for HMIE-NP-B01 and -0.12 ± 0.24‰ (N = 22, 2s) for MAKP-NP-B01, consistent with the solution Fe isotope data. The homogeneity of Fe isotopes of the pellets was evaluated by ns-LA-MC-ICP-MS analyses of three different positions to further confirm that both materials are isotopically homogeneous. Both materials can be considered as potential quality control and bracketing reference materials for Fe isotopic measurements by in situ ns-LA-MC-ICP-MS analysis.
KW - Laser ablation
KW - Fe isotope
KW - Fe-oxides
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654755
DO - https://doi.org/10.1111/ggr.70037
SN - 1639-4488
SP - 1
EP - 12
PB - John Wiley & Sons Ltd.
AN - OPUS4-65475
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Andresen, Elina
A1 - Islam, Fahima
A1 - Prinz, Carsten
A1 - Gehrmann, P.
A1 - Licha, K.
A1 - Roik, Janina
A1 - Recknagel, Sebastian
A1 - Resch-Genger, Ute
T1 - Assessing the reproducibility and up‑scaling of the synthesis of Er,Yb‑doped NaYF4‑based upconverting nanoparticles and control of size, morphology, and optical properties
N2 - Lanthanide-based, spectrally shifting, and multi-color luminescent upconverting nanoparticles (UCNPs) have received much attention in the last decades because of their applicability as reporter for bioimaging, super-resolution microscopy, and sensing as well as barcoding and anti-counterfeiting tags. A prerequisite for the broad application of UCNPs in areas such as sensing and encoding are simple, robust, and easily upscalable synthesis protocols that yield large quantities of UCNPs with sizes of 20 nm or more with precisely controlled and tunable physicochemical properties from lowcost reagents with a high reproducibility. In this context, we studied the reproducibility, robustness, and upscalability of the synthesis of β-NaYF4:Yb, Er UCNPs via thermal decomposition. Reaction parameters included solvent, precursor chemical compositions, ratio, and concentration. The resulting UCNPs were then examined regarding their application-relevant physicochemical properties such as size, size distribution, morphology, crystal phase, chemical composition, and photoluminescence.
Based on these screening studies, we propose a small volume and high-concentration synthesis approach that can provide UCNPs with different, yet controlled size, an excellent phase purity and tunable morphology in batch sizes of up to at least 5 g which are well suited for the fabrication of sensors, printable barcodes or authentication and recycling tags.
KW - Photoluminescence
KW - Nano
KW - Nanomaterial
KW - Synthesis
KW - Reproducibility
KW - Upconversion nanoparticle
KW - Lanthanide
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570170
DO - https://doi.org/10.1038/s41598-023-28875-8
SN - 2045-2322
VL - 13
IS - 1
SP - 1
EP - 13
AN - OPUS4-57017
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Grimmer, Christoph
A1 - Richter, Matthias
A1 - Neuhaus, T.
A1 - Prinz, Carsten
A1 - Strzelczyk, Rebecca Skadi
A1 - Colakoglu, Irem
A1 - Horn, Wolfgang
T1 - Towards a multi-VOC emission reference material with temporally constant emission profile for QA/QC of materials emission testing procedures
N2 - Emission reference materials (ERMs) are sought after to further control and improve indoor air quality. The impregnation of porous materials with volatile organic compounds (VOCs) is a promising approach to produce ERMs. Different VOCs were used to impregnate various porous materials (mainly zeolites, activated carbons and a metal organic framework). The influence of different methodological parameters and material properties were studied to optimize the impregnation procedure and to find the best material/VOC combination. The impregnation procedure remains quite irreproducible, nevertheless, very good ERM candidates were identified. Two materials (zeolite 4 and AC 1 impregnated with n-hexadecane) showed a very stable emission over 14 days (<10 % change). Another material (AC 1 impregnated with toluene) showed a declining emission profile but with a very good in-batch reproducibility and a storage stability of up to 12 months.
KW - Emission reference material
KW - Porous materials
KW - Indoor air quality
KW - Emission test chamber
KW - CO2 assisted impregnation
KW - EN 16516
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612238
DO - https://doi.org/10.1016/j.chemosphere.2024.143437
SN - 1879-1298
VL - 366
SP - 1
EP - 8
PB - Elsevier
AN - OPUS4-61223
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Habibimarkani, Heydar
A1 - Abram, Sarah-Luise
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Prinz, Carsten
A1 - Sahre, Mario
A1 - Hodoroaba, Vasile-Dan
A1 - Radnik, Jörg
T1 - In-depth analysis of FeNi-based nanoparticles for the oxygen evolution reaction
N2 - This study investigates the effect of varying iron-to-nickel ratios on the catalytic performance of Fe-Ni oxide nanoparticles (NPs) for the oxygen evolution reaction (OER). Addressing the issue of high energy wastage due to large overpotentials in OER, we synthesized and characterized different NP catalysts with different Fe: Ni oxide ratios. Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDS), and X-ray Diffraction (XRD) were employed to determine the morphology, elemental and phase composition of the NPs. Furthermore, in-depth profiling with X-ray Photoelectron Spectroscopy (XPS) and Hard X-ray Photoelectron Spectroscopy (HAXPES) revealed that iron predominantly exists as oxide, while nickel exhibits both metallic and oxidic forms depending on the Fe content. XPS indicated an enrichment of iron at the NP surface, whereas HAXPES and EDS data agreed on the bulk stoichiometry. The assessment of the catalytic activity via cyclic voltammetry (CV) showed that the Fe: Ni ratio of 2:3 exhibited superior performance, characterized by lower overpotential and a smaller Tafel slope.
KW - Fe-Ni oxide
KW - Nanoparticles
KW - OER
KW - Catalytic performance
KW - Cyclic voltammetry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626932
UR - https://www.nature.com/articles/s41598-025-92720-3
DO - https://doi.org/10.1038/s41598-025-92720-3
VL - 15
IS - 1
SP - 1
EP - 17
PB - Springer Nature
AN - OPUS4-62693
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Epping, Ruben
A1 - Falkenhagen, Jana
A1 - Panne, Ulrich
A1 - Hiller, W.
A1 - Gruendling, T.
A1 - Staal, B.
A1 - Lang, C.
A1 - Lamprou, A.
T1 - Simultaneous characterization of poly(acrylic acid) andpolysaccharide polymers and copolymers
N2 - Copolymer products that result from grafting acrylic acid and other hydrophilicmonomers onto polysaccharides have recently gained significant interest in researchand industry. Originating from renewable sources, these biodegradable, low toxicity,and polar copolymer products exhibit potential to replace polymers from fossil sourcesin several applications and industries. The methods usually employed to character-ize these copolymers are, however, quite limited, especially for the measurement ofbulk properties. With more sophisticated applications, for example, in pharmaceu-tics requiring a more detailed analysis of the chemical structure, we describe a newapproach for this kind of complex polymers. Our approach utilizes chromatographyin combination with several detection methods to separate and characterize reactionproducts of the copolymerization of acrylic acid and chemically hydrolyzed starch.These samples consisted of a mixture of homopolymer poly (acrylic acid), homopoly-mer hydrolyzed starch, and – in a lower amount – the formed copolymers. Several chro-matographic methods exist that are capable of characterizing either poly (acrylic acid)or hydrolyzed starch. In contrast, our approach offers simultaneous characterization ofboth polymers. The combination of LC and UV/RI offered insight into the compositionand copolymer content of the samples. Size exclusion chromatography experimentsrevealed the molar mass distribution of homopolymers and copolymers. FTIR inves-tigations confirmed the formation of copolymers while ESI-MS gave more details onthe end groups of hydrolyzed starches and poly (acrylic acids). Evidence of copolymerstructures was obtained through NMR measurements. Finally, two-dimensional chro-matography led to the separation of the copolymers from both homopolymers as wellas the additional separation of sodium clusters. The methods described in this work area powerful toolset to characterize copolymerization products of hydrolyzed starch andpoly(acrylic acid). Together, our approach successfully correlates the physicochemicalproperties of such complex mixtures with their actual composition.
KW - 2D chromatography
KW - LC-MS
KW - SEC
KW - Renewable copolymers
KW - Grafting
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508873
DO - https://doi.org/10.1002/ansa.202000044
SP - 1
EP - 12
PB - Wiley-VCH Verlag-GmbH&Co. KGaA
CY - Weinheim
AN - OPUS4-50887
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scholl, Juliane
A1 - Lisec, Jan
A1 - Haase, Hajo
A1 - Koch, Matthias
T1 - Identification of transformation products from fluorinated lithium-ion battery additives TPFPB and TPFPP: forever chemicals of tomorrow?
N2 - AbstractFluorinated organic compounds (FOCs) represent a class of synthetic chemicals distinguished by their resilient carbon–fluorine bonds, which demonstrate an ability to withstand environmental degradation over an extended period. The integration of FOCs into cutting-edge applications, including lithium-ion batteries (LiBs), presents considerable potential for environmental harm that has not yet been sufficiently addressed. This study focuses on the environmental fate of two fluorinated aromatics, tris(pentafluorophenyl)borane (TPFPB) and tris(pentafluorophenyl)phosphine (TPFPP), given their important role in improving the performance of LiBs. To achieve this, laboratory simulation methods including total oxidizable precursor assay, electrochemistry (EC), Fenton reaction, UV-C irradiation, and hydrolysis were employed. Liquid chromatography and gas chromatography coupled with high-resolution mass spectrometry were used for identification of transformation products (TPs) and prediction of their molecular formulae. Despite the structural similarity between TPFPB and TPFPP, distinct differences in electrochemical behavior and degradation pathways were observed. TPFPB readily underwent hydroxylation and hydrolysis, resulting in a wide range of 49 TPs. A total of 28 TPs were newly identified, including oligomers and highly toxic dioxins. In contrast, TPFPP degraded exclusively under harsh conditions, requiring the development of innovative conditioning protocols for EC. In total, the simulation experiments yielded nine structurally different compounds, including seven previously undescribed, partially defluorinated TPs. This study highlights the potential risks associated with the use of FOCs in LiBs and provides insight into the complex environmental behavior of FOCs.
KW - Mass Spectrometry
KW - LiBs
KW - POPs
KW - Transformation products
KW - Electrochemistry
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611339
DO - https://doi.org/10.1007/s00216-024-05526-z
SP - 1
EP - 15
PB - Springer Science and Business Media LLC
AN - OPUS4-61133
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Meiers, Emelie
A1 - Scholl, Juliane
A1 - Droas, Morten
A1 - Vogel, Christian
A1 - Leube, Peter
A1 - Sommerfeld, Thomas
A1 - Bagheri, A.
A1 - Adam, Christian
A1 - Seubert, A.
A1 - Koch, Matthias
T1 - Development and evaluation of analytical strategies for the monitoring of per- and polyfluoroalkyl substances from lithium-ion battery recycling materials
N2 - Per- and polyfluoroalkyl substances (PFAS) are well-known as “forever chemicals” and persistent pollutants released by different anthropogenic sources. The potential release of PFAS from accumulating electronic waste and lithium-ion battery (LIB) recycling activities has gained increasing attention in the past years. This creates a need for analytical methods tailored for the determination of PFAS out of environmental matrices related to the named activities or directly out of the concerned materials. In this work, analytical strategies for the monitoring of PFAS in LIB recycling materials were explored for a group of legacy perfluoro sulfonic- and carbonic acids (PFSA and PFCA) and of fluorinated sulfonylimides suspected to be LIB electrolyte ingredients. These analytical strategies comprehend PFAS target approaches with a herein optimized liquid chromatography tandem mass spectrometry (LC–MS/MS) method equipped with a HILIC (hydrophilic interaction liquid chromatography) column in combination with the TOP (total oxidizable precursor) assay and an adapted sample preparation method for high-matrix LIB recycling materials. The validated target method was applied to a set of LIB recycling materials: end-of-life batteries, black masses from hydrometallurgical recycling, and gas absorption solutions from thermal treatment of black masses as part of the recycling procedure. Investigation results show that the LIB industry can be connected to the release of both “LIB”-PFAS, such as the target sulfonylimides, and “already-legacy” PFAS, like the PFSA and PFCA. Especially, the presence of trifluoroacetic acid (TFA) as an emerging pollutant in every investigated LIB material type underlines the threat of PFAS emissions from LIB waste and recycling activities.
KW - Per- and polyfluoroalkyl substances (PFAS)
KW - Battery
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647015
DO - https://doi.org/10.1007/s00216-025-06165-8
SN - 1618-2642
VL - 417
SP - 6567
EP - 6583
PB - Springer Science and Business Media LLC
AN - OPUS4-64701
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scholl, Juliane
A1 - Lisec, Jan
A1 - Bagheri, Abbas
A1 - Meiers, Emelie
A1 - Russo, Francesco Friedrich
A1 - Haase, Hajo
A1 - Koch, Matthias
T1 - Unveiling aging mechanisms of electrolytes in commercial end-of-life lithium-ion batteries
N2 - In this study, 77 end-of-life (EOL) commercial lithium-ion batteries (LIBs) of various formats were systematically analyzed to investigate electrolyte degradation and the influence of pristine electrolyte compositions on aging behavior. Comprehensive chemical characterization was conducted using targeted and non-targeted mass spectrometry (MS), employing LC-MS/MS, GC-MS, and high-resolution MS (HRMS). This integrated approach enabled the identification of confirmed pristine components and complex degradation products. The results show that rechargeable pouch and cylindrical cells often deviate from conventional model systems, containing mixed lithium salt anions, ionic liquids (ILs), and high concentrations of triflates, triflimides, and bis(fluorosulfonyl)imide (FSI). These function as solvents, salts, or safety-enhancing additives. Specific IL degradation products were identified, and hypotheses formulated on previously unreported pathways. Furthermore, a novel series of oligomerization products of propylene carbonate (PC) was detected. In contrast, non-rechargeable coin cells revealed widespread use of per- and polyfluoroalkyl substances (PFAS) in their original electrolytes. Based on ex situ analyses, hypothetical PFAS degradation mechanisms are proposed here for the first time. The absence of carbonate oligomers and lithium salt-derived products, alongside the presence of standard carbonates, indicates lithium counterion coordination as a key factor in Lewis acid-catalyzed degradation. This study offers valuable insights into real-world battery aging.
KW - Transformation products
KW - Lithium-ion batteries
KW - Fluorinated Compounds
KW - Gas chromatography/ QTOF-MS
KW - HILIC-LC-MS/MS
KW - PFAS
KW - Electrochemistry
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644991
DO - https://doi.org/10.1016/j.jpowsour.2025.238613
SN - 0378-7753
VL - 661
SP - 1
EP - 10
PB - Elsevier B.V.
AN - OPUS4-64499
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Prakash, Swayam
A1 - Bell, Jérémy
A1 - Rurack, Knut
T1 - Rapid Onsite Detection of Fecal Contamination in Water Using a Portable Fluorometric Assay
N2 - Fecal pollution in water poses significant health risks, especially when contaminated sources are used for drinking and food production. Traditional water quality testing methods are expensive, slow, and require skilled personnel, limiting their accessibility. This work addresses these issues by developing a portable fluorometric assay for the detection of the fecal indicator pigment urobilin (UB). The assay uses silane-functionalized glass fiber strips impregnated with zinc chloride, providing a ‘drop-&-detect’ approach with enhanced fluorescence response mediated by the unique complexation properties of ZnCl2 and UB. This approach allows for the detection of UB at sub-nanomolar concentrations in less than 1 min using a 3D-printed setup with miniaturized optical components powered by a smartphone with its camera as a detector. The results validated with a benchtop fluorometer show the effectiveness of this method. The successful application of this userfriendly, rapid, and sensitive assay to real water samples from three rivers and the influx and efflux of a wastewater treatment plant advances field-based water quality monitoring, meets the WHO’s ASSURED criteria, and supports progress toward the global clean water and sanitation goals.
KW - Fecal pigment
KW - Fluorescence
KW - Signal amplification
KW - Surface chemistry
KW - Water quality testing
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655543
DO - https://doi.org/10.1021/acssensors.5c03922
SN - 2379-3694
VL - 11
SP - 1
EP - 9
PB - American Chemical Society
CY - Washington, D.C.
AN - OPUS4-65554
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lisec, Jan
A1 - Recknagel, Sebastian
A1 - Prinz, Carsten
A1 - Vogel, Kristin
A1 - Koch, Matthias
A1 - Becker, Roland
T1 - eCerto—versatile software for interlaboratory data evaluation and documentation during reference material production
N2 - The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials.
KW - Reference material
KW - Statistics
KW - Software
KW - Collaborative trial
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591851
DO - https://doi.org/10.1007/s00216-023-05099-3
SP - 1
EP - 9
PB - Springer Science and Business Media LLC
AN - OPUS4-59185
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gerrits, Ruben
A1 - Stepec, Biwen An
A1 - Bäßler, Ralph
A1 - Becker, Roland
A1 - Dimper, Matthias
A1 - Feldmann, Ines
A1 - Goff, Kira L.
A1 - Günster, Jens
A1 - Hofmann, Andrea
A1 - Hesse, René
A1 - Kirstein, Sarah
A1 - Klein, Ulrich
A1 - Mauch, Tatjana
A1 - Neumann-Schaal, Meina
A1 - Özcan Sandikcioglu, Özlem
A1 - Taylor, Nicole M.
A1 - Schumacher, Julia
A1 - Shen, Yin
A1 - Strehlau, Heike
A1 - Weise, Matthias
A1 - Wolf, Jacqueline
A1 - Yurkov, Andrey
A1 - Gieg, Lisa M.
A1 - Gorbushina, Anna
T1 - A 30-year-old diesel tank: Fungal-dominated biofilms cause local corrosion of galvanised steel
N2 - The increased use of biodiesel is expected to lead to more microbial corrosion, fouling and fuel degradation issues. In this context, we have analysed the metal, fuel and microbiology of a fouled diesel tank which had been in service for over 30 years. The fuel itself, a B7 biodiesel blend, was not degraded, and—although no free water phase was visible—contained a water content of ~60 ppm. The microbial community was dominated by the fungus Amorphotheca resinae, which formed thick, patchy biofilms on the tank bottom and walls. The tank sheets, composed of galvanised carbon steel, were locally corroded underneath the biofilms, up to a depth of a third of the sheet thickness. On the biofilm-free surfaces, Zn coatings could still be observed. Taken together, A. resinae was shown to thrive in these water-poor conditions, likely enhancing corrosion through the removal of the protective Zn coatings.
KW - Fungal biofilms
KW - Biodiesel degradation mechanisms
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655014
DO - https://doi.org/10.1038/s41529-025-00731-2
SN - 2397-2106
VL - 10
IS - 1
SP - 1
EP - 14
PB - Springer Science and Business Media LLC
AN - OPUS4-65501
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sichler, Theresa Constanze
A1 - Adam, Christian
A1 - Barjenbruch, M.
A1 - Montag, D.
A1 - Mauch, Tatjana
A1 - Sommerfeld, Thomas
A1 - Ehm, J.H.
T1 - Variation of the element composition of municipal sewage sludges in the context of new regulations on phosphorus recovery in Germany
N2 - Phosphorus (P) recovery is obligatory for all sewage sludges with more than 20 g P/kg dry matter (DM) from 2029 in Germany. Nine wastewater treatment plants (WWTPs) were chosen to investigate variations of phosphorus contents and other parameters in sewage sludge over the year. Monthly sewage sludge samples from each WWTP were analyzed for phosphorus and other matrix elements (C, N, H, Ca, Fe, Al, etc.), for several trace elements (As, Cr, Mo, Ni, Pb, Sn) and loss of ignition. Among the nine WWTPs, there are four which have phosphorus contents both above and below the recovery limit of 20 g/kg DM along the year. Considering the average phosphorus content over the year, only one of them is below the limit. Compared to other matrix elements and parameters, phosphorus fuctuations are low with an average of 7% over all nine WWTPs. In total, only hydrogen and carbon are more constant in the sludge.
In several WWTPs with chemical phosphorus elimination, phosphorus fuctuations showed similar courses like iron and/or aluminum. WWTPs with chamber flter presses rather showed dilution efects of calcium dosage. As result of this study, monthly phosphorus measurement is highly recommended to determine whether a WWTP is below the
20 g/kg DM limit.
KW - Sewage sludge
KW - Phosphorus recovery
KW - Wastewater
KW - Phosphorus elimination
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557499
DO - https://doi.org/10.1186/s12302-022-00658-4
SN - 2190-4707
VL - 34
IS - 1
SP - 1
EP - 12
PB - Springer Nature
CY - Berlin
AN - OPUS4-55749
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wetzel, Annica
A1 - Morell, Daniel
A1 - von der Au, Marcus
A1 - Witt, Julia
A1 - Özcan Sandikcioglu, Özlem
T1 - Transpassive Behavior of Equimolar CrMnFeCoNi and CrCoNi Multi‐Principal Element Alloys in an Alkaline NaCl Electrolyte
N2 - AbstractWe investigated the corrosion properties and transpassive behavior of CrMnFeCoNi and CrCoNi multi‐principal element alloys (MPEAs) in a 0.1 M NaCl electrolyte at pH 12. By using SECM‐based tip substrate voltammetry (TSV) in combination with the chemical analysis of the electrolyte, we were able to differentiate between anodic metal dissolution and oxygen evolution in the transpassive range. Our investigations have shown that CrCoNi has a significantly higher corrosion resistance compared to CrMnFeCoNi. In the studied alkaline environment, a transpassive oxide film is formed on the surface of CrCoNi during secondary passivation. This transpassive oxide film appears to play a significant role in oxygen evolution, as the increase in TSV currents at the microelectrode coincides with the corresponding current density plateau of the voltametric current trace. The formation of the transpassive oxide film was not observed in previous studies conducted in acidic environments. Moreover, the alkaline electrolyte induced a positive hysteresis and mild pitting corrosion, in addition to intergranular corrosion, which was the sole corrosion process observed at acidic pH levels. These findings enhance the understanding of the processes governing the transpassivity of CrMnFeCoNi and CrCoNi MPEAs in alkaline environments and have potential implications for the development of application‐tailored corrosion‐resistant MPEAs.
KW - Multi-principal element alloys
KW - MPEA
KW - Corrosion
KW - Oxygen evolution reaction
KW - Transpassive region
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611594
DO - https://doi.org/10.1002/celc.202400346
SN - 2196-0216
SP - 1
EP - 9
PB - Wiley
AN - OPUS4-61159
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Recknagel, Sebastian
A1 - Richter, Silke
A1 - Hoppe, Marion
A1 - Meckelburg, Angela
A1 - Prinz, Carsten
A1 - Roik, Janina
A1 - Abad Andrade, Carlos Enrique
T1 - Powering precision: development of a certified reference material for elemental composition analysis of lithium nickel manganese cobalt oxide (Li-NMC) cathode material for lithium-ion batteries
N2 - This work presents the development and certification of the world’s first certified reference material (CRM), BAM-S014, for a lithium nickel manganese cobalt oxide (LiNi0.33Mn0.33Co0.33O2 or Li-NMC 111) cathode material—an integral component in high-energy-density lithium-ion batteries that power electric vehicles (EVs), portable electronics, and stationary energy storage systems. By providing certified mass fractions for 11 elements, this CRM addresses a critical need for accurate and traceable elemental analysis, supporting quality control and regulatory compliance in the global battery industry. Ensuring reliable and harmonized measurements supports the efficient use of resources, including the reuse of recycled materials, and ultimately helps maintain product performance and safety. The values were assigned through an interlaboratory comparison involving 16 participating laboratories and various analytical techniques such as inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence (XRF) spectrometry, and combustion analysis. In addition to chemical characterization, the certification process includes homogeneity and stability testing of the candidate material. Details are provided on the analytical methods used for chemical characterization and the calculation of the uncertainties of the certified mass fractions. In addition to detailing the development of the CRMs, this work provides an overview of ongoing standardization activities in Li-component analysis, thereby guiding the calibration of analytical methods and contributing to the establishment of globally accepted standards for evaluating energy storage materials and advancing sustainable mobility and clean energy solutions.
KW - Certified reference material
KW - Lithium nickel manganese cobalt oxide
KW - LNMC
KW - Lithium-ion battery
KW - Cathode material
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643763
DO - https://doi.org/10.1007/s00216-025-05766-7
SN - 1618-2642
VL - 417
IS - 12
SP - 2643
EP - 2653
PB - Springer Nature
AN - OPUS4-64376
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 - JOUR
A1 - Kossatz, Philipp
A1 - Mezhov, Alexander
A1 - Andresen, Elina
A1 - Prinz, Carsten
A1 - Schmidt, Wolfram
A1 - Resch-Genger, Ute
T1 - Assessing the Applicability of Lanthanide-Based Upconverting Nanoparticles for Optically Monitoring Cement Hydration and Tagging Building Materials
N2 - Chemically stable, lanthanide-based photon upconversion micro- and nanoparticles (UCNPs) with their characteristic multicolor emission bands in the ultraviolet (UV), visible (vis), near-infrared (NIR), and short-wave infrared (SWIR) arepromising optical reporters and barcoding tags. To assess the applicability of UCNPs for the monitoring of early stage cement hydration processes and as authentication tags for cementitious materials, we screened the evolution of the luminescence of Selfmade core-only NaYF4:Yb,Er UCNPs and commercial μm-sized Y2O2S:Yb,Er particles during the first stages of cement hydration, which largely determines the future properties of the hardened material. Parameters explored from the UCNP side included particle size, morphology, surface chemistry or coating, luminescence properties, and concentration in different cement mixtures. From the cement side, the influence of the mineral composition of the cement matrix was representatively examined for ordinary Portland cement (OPC) and its constituents tricalcium aluminate (C3A), tricalcium silicate (C3S), and gypsum at different water to cement ratios. Based on reflection and luminescence measurements, enabling online monitoring, which were complemented by XRD and isothermal heat-flow calorimetric measurements to determine whether the incorporation of these particles could impair cement hydration processes, well suited lanthanide particle reporters could be identified as well as application conditions. In addition, thereby the reporter influence on cement hydration kinetics could be minimized while still preserving a high level of information content. The best performance for the luminescence probing of changes during early stage cement hydration processes was observed for 25 nm-sized oleate (OA)-coated UCNPs added in a concentration of 0.1 wt %. Higher UCNP amounts of 1.0 wt % delayed cement hydration processes size- and surface coatingspecifically in the first 24 h. Subsequent luminescence stability screening studies performed over a period of about one year support the applicability of UCNPs as optical authentication tags for construction materials.
KW - Quality assurance
KW - Fluorescence
KW - Nano
KW - Particle
KW - Synthesis
KW - Quantum yield
KW - NIR
KW - Mechanism
KW - Characterization
KW - XRD
KW - Calorimetry
KW - Advanced material
KW - Cement
KW - Monitoring
KW - Surface
KW - Size
KW - Lifetime
KW - Barcode
KW - Lanthanide
KW - Upconversion
KW - Encoding
KW - Method
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638318
DO - https://doi.org/10.1021/acsomega.5c02236
SN - 2470-1343
VL - 10
IS - 29
SP - 31587
EP - 31599
PB - ACS Publications
CY - Washington, DC
AN - OPUS4-63831
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dhamo, Lorena
A1 - Wegner, Karl David
A1 - Würth, Christian
A1 - Häusler, I.
A1 - Hodoroaba, Vasile-Dan
A1 - Resch-Genger, Ute
T1 - Assessing the influence of microwave-assisted synthesis parameters and stabilizing ligands on the optical properties of AIS/ZnS quantum dots
N2 - Luminescent semiconductor quantum dots (QDs) are frequently used in the life and material sciences as reporter for bioimaging studies and as active components in devices such as displays, light-emitting diodes, solar cells, and sensors. Increasing concerns regarding the use of toxic elements like cadmium and lead, and hazardous organic solvents during QD synthesis have meanwhile triggered the search for heavy-metal free QDs using green chemistry syntheses methods. Interesting candidates are ternary AgInS2 (AIS) QDs that exhibit broad photoluminescence (PL) bands, large effective Stokes shifts, high PL quantum yields (PL QYs), and long PL lifetimes, which are particularly beneficial for applications such as bioimaging, white light-emitting diodes, and solar concentrators. In addition, these nanomaterials can be prepared in high quality with a microwave-assisted (MW) synthesis in aqueous solution. The homogeneous heat diffusion and instant temperature rise of the MW synthesis enables a better control of QD nucleation and growth and thus increases the batch-to-batch reproducibility. In this study, we systematically explored the MW synthesis of AIS/ZnS QDs by varying parameters such as the order of reagent addition, precursor concentration, and type of stabilizing thiol ligand, and assessed their influence on the optical properties of the resulting AIS/ZnS QDs. Under optimized synthesis conditions, water-soluble AIS/ZnS QDs with a PL QY of 65% and excellent colloidal and long-term stability could be reproducible prepared.
KW - Quantum dots
KW - Microwave-assisted synthesis
KW - AgInS
KW - Aqueous synthesis
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567091
DO - https://doi.org/10.1038/s41598-022-25498-3
SN - 2045-2322
VL - 12
IS - 1
SP - 1
EP - 11
PB - Nature Publishing Group
CY - London
AN - OPUS4-56709
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hülagü, Deniz
A1 - Tobias, Charlie
A1 - Dao, Radek
A1 - Komarov, Pavel
A1 - Rurack, Knut
A1 - Hodoroaba, Vasile-Dan
T1 - Towards 3D determination of the surface roughness of core–shell microparticles as a routine quality control procedure by scanning electron microscopy
N2 - AbstractRecently, we have developed an algorithm to quantitatively evaluate the roughness of spherical microparticles using scanning electron microscopy (SEM) images. The algorithm calculates the root-mean-squared profile roughness (RMS-RQ) of a single particle by analyzing the particle’s boundary. The information extracted from a single SEM image yields however only two-dimensional (2D) profile roughness data from the horizontal plane of a particle. The present study offers a practical procedure and the necessary software tools to gain quasi three-dimensional (3D) information from 2D particle contours recorded at different particle inclinations by tilting the sample (stage). This new approach was tested on a set of polystyrene core-iron oxide shell-silica shell particles as few micrometer-sized beads with different (tailored) surface roughness, providing the proof of principle that validates the applicability of the proposed method. SEM images of these particles were analyzed by the latest version of the developed algorithm, which allows to determine the analysis of particles in terms of roughness both within a batch and across the batches as a routine quality control procedure. A separate set of particles has been analyzed by atomic force microscopy (AFM) as a powerful complementary surface analysis technique integrated into SEM, and the roughness results have been compared.
KW - Core–shell particles
KW - Image analysis
KW - Roughness
KW - Scanning electron microscopy
KW - Atomic force microscopy
KW - Tilting
KW - Batch analysis
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607590
DO - https://doi.org/10.1038/s41598-024-68797-7
SN - 2045-2322
VL - 14
IS - 1
SP - 1
EP - 13
PB - Springer Science and Business Media LLC
AN - OPUS4-60759
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 - Dhamo, Lorena
A1 - Carulli, F.
A1 - Nickl, Philip
A1 - Wegner, Karl David
A1 - Hodoroaba, Vasile-Dan
A1 - Würth, Christian
A1 - Brovelli, S.
A1 - Resch-Genger, Ute
T1 - Efficient luminescent solar concentrators based on environmentally friendly Cd-free ternary AIS/ZnS quantum dots
N2 - Luminescent solar concentrators (LSC) allow to obtain renewable energy from building integrated photovoltaic systems. As promising efficient and long-term stable LSC fluorophores semiconductor nanocrystals like Quantum dots (QDs) with size and composition tunable optoelectronic properties have recently emerged. The most popular II/VI or IV/VI semiconductor QDs contain, however, potentially hazardous cadmium or lead ions, which is a bottleneck for commercial applications. A simple aqueous based, microwaveassisted synthesis for environmentally friendly and highly emissive AgInS2/ ZnS QDs is developed using 3-mercaptopropionic acid (MPA) and glutathione (GSH) and their incorporation into polylaurylmethacrylate (PLMA) polymer slabs integrable in LSC devices (10.4 × 10.4 × 0.2 cm3, G = 12.98).
With this simple approach, optical power efficiencies (OPE) of 3.8% and 3.6% and optical quantum efficiencies (OQE) of 24.1% and 27.4% are obtained, which are among the highest values yet reported.
KW - Solar energy
KW - Solar concentrator
KW - Quantum dots
KW - Advanced material
KW - Quantum yield
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529735
DO - https://doi.org/10.1002/adom.202100587
SN - 2195-1071
SN - 0935-9648
VL - 9
IS - 17
SP - 1
EP - 8
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-52973
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rühle, Bastian
A1 - Krumrey, Julian Frederic
A1 - Hodoroaba, Vasile-Dan
T1 - Workflow towards automated segmentation of agglomerated, non‑spherical particles from electron microscopy images using artificial neural networks
N2 - We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from scanning electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. We compare the segmentation masks obtained with our suggested workflow qualitatively and quantitatively to state-of-the-art methods using various metrics. Finally, we used the segmentation masks for automatically extracting particle size distributions from the SEM images of TiO2 particles, which were in excellent agreement with particle size distributions obtained manually but could be obtained in a fraction of the time.
KW - Electron microscopy
KW - Neural networks
KW - Artificial intelligence
KW - Image segmentation
KW - Automated image analysis
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522454
DO - https://doi.org/10.1038/s41598-021-84287-6
VL - 11
IS - 1
SP - 4942
PB - Springer Nature
AN - OPUS4-52245
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zhang, Kun
A1 - Carrod, Andrew J.
A1 - Del Giorgio, Elena
A1 - Hughes, Joseph
A1 - Rurack, Knut
A1 - Bennet, Francesca
A1 - Hodoroaba, Vasile-Dan
A1 - Harrad, Stuart
A1 - Pikramenou, Zoe
T1 - Luminescence Lifetime-Based Sensing Platform Based on Cyclometalated Iridium(III) Complexes for the Detection of Perfluorooctanoic Acid in Aqueous Samples
N2 - Luminescence lifetimes are an attractive analytical method for detection due to its high sensitivity and stability. Iridium probes exhibit luminescence with long excited-state lifetimes, which are sensitive to the local environment. Perfluorooctanoic acid (PFOA) is listed as a chemical of high concern regarding its toxicity and is classified as a “forever chemical”. In addition to strict limits on the presence of PFOA in drinking water, environmental contamination from industrial effluent or chemical spills requires rapid, simple, accurate, and cost-effective analysis in order to aid containment. Herein, we report the fabrication and function of a novel and facile luminescence sensor for PFOA based on iridium modified on gold surfaces. These surfaces were modified with lipophilic iridium complexes bearing alkyl chains, namely, IrC6 and IrC12, and Zonyl-FSA surfactant. Upon addition of PFOA, the modified surfaces IrC6-FSA@Au and IrC12-FSA @Au show the largest change in the red luminescence signal with changes in the luminescence lifetime that allow monitoring of PFOA concentrations in aqueous solutions. The platform was tested for the measurement of PFOA in aqueous samples spiked with known concentrations of PFOA and demonstrated the capacity to determine PFOA at concentrations >100 μg/L (240 nM).
KW - Perfluorooctanoic Acid (PFOA)
KW - Cyclometalated iridium (III) complexes
KW - Luminescent lifetime
KW - Optically active surfaces
KW - ToF-SIMS
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594535
UR - https://pubs.acs.org/doi/10.1021/acs.analchem.3c04289
DO - https://doi.org/10.1021/acs.analchem.3c04289
VL - 96
IS - 4
SP - 1565
EP - 1575
PB - American Chemical Society (ACS)
AN - OPUS4-59453
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hülagü, Deniz
A1 - Tobias, Charlie
A1 - Climent Terol, Estela
A1 - Gojani, Ardian
A1 - Rurack, Knut
A1 - Hodoroaba, Vasile-Dan
T1 - Generalized Analysis Approach of the Profile Roughness by Electron Microscopy with the Example of Hierarchically Grown Polystyrene–Iron Oxide–Silica Core–Shell–Shell Particles
N2 - The roughness as a property of core–shell (CS) microparticles plays a key role in their functionality. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task with approaches using electron microscopy images being scarce and showing pronounced differences in terms of methodology and results. This work presents a generalized method for the reliable roughness determination of nonplanar specimens such as CS particles from electron microscopic images, the method being robust and reproducible with a high accuracy. It involves a self-written software package (Python) that analyzes the recorded images, extracts corresponding data, and calculates the roughness based on the deviation of the identified contour. Images of single particles are taken by a dual mode scanning electron microscopy (SEM) setup which permits imaging of the same field-of-view of the sample with high resolution and surface sensitive in SE InLens mode as well as in transmission mode (TSEM). Herein, a new type of polystyrene core–iron oxide shell–silica shell particles is developed to serve as a set of lower micrometer-sized study objects with different surface roughness; the analysis of their images by the semiautomatic workflow is demonstrating that the particles’ profile roughness can be quantitatively obtained.
KW - Core–shell particles
KW - Image analysis
KW - Nanoparticles
KW - Roughness
KW - SEM
KW - transmission mode
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542576
DO - https://doi.org/10.1002/adem.202101344
SP - 1
EP - 9
PB - Wiley-VCH
AN - OPUS4-54257
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Bayerlein, Bernd
A1 - Hanke, T.
A1 - Muth, Thilo
A1 - Riedel, Jens
A1 - Schilling, Markus
A1 - Schweizer, C.
A1 - Skrotzki, Birgit
A1 - Todor, A.
A1 - Moreno Torres, Benjami
A1 - Unger, Jörg F.
A1 - Völker, Christoph
A1 - Olbricht, Jürgen
T1 - A Perspective on Digital Knowledge Representation in Materials Science and Engineering
N2 - The amount of data generated worldwide is constantly increasing. These data come from a wide variety of sources and systems, are processed differently, have a multitude of formats, and are stored in an untraceable and unstructured manner, predominantly in natural language in data silos. This problem can be equally applied to the heterogeneous research data from materials science and engineering. In this domain, ways and solutions are increasingly being generated to smartly link material data together with their contextual information in a uniform and well-structured manner on platforms, thus making them discoverable, retrievable, and reusable for research and industry. Ontologies play a key role in this context. They enable the sustainable representation of expert knowledge and the semantically structured filling of databases with computer-processable data triples.
In this perspective article, we present the project initiative Materials-open-Laboratory (Mat-o-Lab) that aims to provide a collaborative environment for domain experts to digitize their research results and processes and make them fit for data-driven materials research and development. The overarching challenge is to generate connection points to further link data from other domains to harness the promised potential of big materials data and harvest new knowledge.
KW - Data infrastructures
KW - Digital representations
KW - Digital workflows
KW - Knowledge graphs
KW - Materials informatics
KW - Ontologies
KW - Vocabulary providers
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546729
DO - https://doi.org/10.1002/adem.202101176
SN - 1438-1656
SP - 1
EP - 14
PB - Wiley-VCH GmbH
CY - Weinheim
AN - OPUS4-54672
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Braymer, Joseph J.
A1 - Knauer, Lukas
A1 - Crack, Jason C.
A1 - Oltmanns, Jonathan
A1 - Heghmanns, Melanie
A1 - Soares, Jéssica C.
A1 - Le Brun, Nick E.
A1 - Schünemann, Volker
A1 - Kasanmascheff, Müge
T1 - Yeast [FeFe]-hydrogenase-like protein Nar1 binds a [2Fe–2S] cluster
N2 - Nar1 is an essential eukaryotic protein proposed to function as an iron–sulphur (Fe/S) cluster trafficking factor in the cytosolic iron–sulphur protein assembly (CIA) machinery. However, such a role has remained unclear due to difficulties in purifying adequate amounts of cofactor-bound protein. The [FeFe]-hydrogenase-like protein has two conserved binding sites for [4Fe–4S] clusters but does not show hydrogenase activity in vivo due to the lack of an active site [2Fe]H cofactor. Here, we report a new preparation procedure for Nar1 that facilitated studies by UV-vis, EPR, and Mössbauer spectroscopies, along with native mass spectrometry. Nar1 recombinantly produced in E. coli contained a [4Fe–4S] cluster, bound presumably at site 1, along with an unexpected [2Fe–2S] cluster bound at an unknown site. Fe/S reconstitution reactions installed a second [4Fe–4S] cluster at site 2, leading to protein with up to three Fe/S cofactors. It is proposed that the [2Fe–2S] cluster occupies a cavity in Nar1 that is filled by the [2Fe]H cofactor in [FeFe]-hydrogenases. Strikingly, two of the Fe/S clusters were rapidly destroyed by molecular oxygen, linking Nar1 oxygen sensitivity in vitro to phenotypes observed previously in vivo. Our biochemical results, therefore, validate a direct link between cellular oxygen concentrations and the functioning of the CIA pathway. These advances also now allow for the pursuit of in vitro Fe/S cluster transfer assays, which will shed light on Fe/S trafficking and insertion by CIA components.
KW - Biocorrosion
KW - Hydrogenases
KW - Metalloprotein
KW - Yeast
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649463
DO - https://doi.org/10.1039/D5SC04860E
SN - 2041-6520
VL - 17
IS - 1
SP - 373
EP - 380
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64946
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Saleh, Maysoon I.
A1 - Rühle, Bastian
A1 - Wang, Shu
A1 - Radnik, Jörg
A1 - You, Yi
A1 - Resch-Genger, Ute
T1 - Assessing the protective effects of different surface coatings on NaYF4:YB3+, Er3+, upconverting nanoparticles in buffer and DMEM
N2 - We studied the dissolution behavior of β NaYF4:Yb(20%), Er(2%) UCNP of two different sizes in biologically relevant media i.e., water (neutral pH), phosphate buffered saline (PBS), and Dulbecco’s modified Eagle medium (DMEM) at different temperatures and particle concentrations. Special emphasis was dedicated to assess the influence of different surface functionalizations, particularly the potential of mesoporous and microporous silica shells of different thicknesses for UCNP stabilization and protection. Dissolution was quantified electrochemically using a fluoride ion selective electrode (ISE) and by inductively coupled plasma optical emission spectrometry (ICP OES). In addition, dissolution was monitored fluorometrically. These experiments revealed that a thick microporous silica shell drastically decreased dissolution. Our results also underline the critical influence of the chemical composition of the aqueous environment on UCNP dissolution. In DMEM, we observed the formation of a layer of adsorbed molecules on the UCNP surface that protected the UCNP from dissolution and enhanced their fluorescence. Examination of this layer by X ray photoelectron spectroscopy (XPS) and mass spectrometry (MS) suggested that mainly phenylalanine, lysine, and glucose are adsorbed from DMEM. These findings should be considered in the future for cellular toxicity studies with UCNP and other nanoparticles and the design of new biocompatible surface coatings.
KW - Fluorescence
KW - Lifetime
KW - Method
KW - Quantification
KW - Stability
KW - Coating
KW - Surface chemistry
KW - Lanthanide
KW - Fluoride
KW - Electrochemistry
KW - ICP-OES
KW - Upconversion
KW - Nano
KW - Particle
KW - Aging
KW - Quality assurance
KW - Mass spectrometry
KW - XPS
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515984
DO - https://doi.org/10.1038/s41598-020-76116-z
SN - 2045-2322
VL - 10
IS - 1
SP - 19318-1
EP - 19318-11
PB - Springer Nature
CY - London
AN - OPUS4-51598
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Cairns, Warren R. L.
A1 - Braysher, Emma C.
A1 - Butler, Owen T.
A1 - Cavoura, Olga
A1 - Davidson, Christine M.
A1 - Todoli Torro, Jose Luis
A1 - von der Au, Marcus
T1 - Atomic spectrometry update: review of advances in environmental analysis
N2 - This review covers advances in the analysis of air, water, plants, soils and geological materials by a range of atomic spectrometric techniques including atomic emission, absorption, fluorescence and mass spectrometry.
KW - Environmental analysis
KW - Review
KW - Trend Article
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653977
DO - https://doi.org/10.1039/D5JA90058A
SN - 0267-9477
VL - 41
IS - 1
SP - 16
EP - 70
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65397
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 -
TY - JOUR
A1 - Srivastava, Priyanka
A1 - Tavernaro, Isabella
A1 - Scholtz, Lena
A1 - Genger, C.
A1 - Welker, P.
A1 - Schreiber, Frank
A1 - Meyer, Klas
A1 - Resch-Genger, Ute
T1 - Dual color pH probes made from silica and polystyrene nanoparticles and their performance in cell studies
N2 - Ratiometric green–red fluorescent nanosensors for fluorometrically monitoring pH in the acidic range were designed from 80 nm-sized polystyrene (PS) and silica (SiO2) nanoparticles (NPs), red emissive reference dyes, and a green emissive naphthalimide pH probe, analytically and spectroscopically characterized, and compared regarding their sensing performance in aqueous dispersion and in cellular uptake studies. Preparation of these optical probes, which are excitable by 405 nm laser or LED light sources, involved the encapsulation of the pH-inert red-fuorescent dye Nile Red (NR) in the core of self-made carboxylated PSNPs by a simple swelling procedure and the fabrication of rhodamine B (RhB)-stained SiO2-NPs from a silane derivative of pH-insensitive RhB. Subsequently, the custom-made naphthalimide pH probe, that utilizes a protonation-controlled photoinduced electron transfer process, was covalently attached to the carboxylic acid groups at the surface of both types of NPs. Fluorescence microscopy studies with the molecular and nanoscale optical probes and A549 lung cancer cells confirmed the cellular uptake of all probes and their penetration into acidic cell compartments, i.e., the lysosomes, indicated by the switching ON of the green naphthalimide fluorescence. This underlines their suitability for intracellular pH sensing, with the SiO2-based nanosensor revealing the best performance regarding uptake speed and stability.
KW - Sensors
KW - Silica and polystyrene nanoparticles
KW - pH probe
KW - Fluorescence spectroscopy
KW - Cell studies
KW - Dye
KW - Particle synthesis
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569198
DO - https://doi.org/10.1038/s41598-023-28203-0
SN - 2045-2322
VL - 13
IS - 1
SP - 1321
EP - 1336
PB - Nature
CY - London
AN - OPUS4-56919
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Nordholt, Niclas
A1 - O'Hara, Kate
A1 - Resch-Genger, Ute
A1 - Blaskovich, M.
A1 - Rühle, Bastian
A1 - Schreiber, Frank
T1 - A fluorescently labelled quaternary ammonium compound (NBD-DDA) to study resistance mechanisms in bacteria
N2 - Quaternary ammonium compounds (QACs) are widely used as active agents in disinfectants, antiseptics, and preservatives. Despite being in use since the 1940s, there remain multiple open questions regarding their detailed mode-of-action and the mechanisms, including phenotypic heterogeneity, that can make bacteria less susceptible to QACs. To facilitate studies on resistance mechanisms towards QACs, we synthesized a fluorescent quaternary ammonium compound, namely N-dodecyl-N,N-dimethyl-[2-[(4-nitro-2,1,3-benzoxadiazol-7-yl)amino]ethyl]azanium-iodide (NBD-DDA). NBD-DDA is readily detected by flow cytometry and fluorescence microscopy with standard GFP/FITC-settings, making it suitable for molecular and single-cell studies. As a proof-of-concept, NBD-DDA was then used to investigate resistance mechanisms which can be heterogeneous among individual bacterial cells. Our results reveal that the antimicrobial activity of NBD-DDA against Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa is comparable to that of benzalkonium chloride (BAC), a widely used QAC, and benzyl-dimethyl-dodecylammonium chloride (BAC12), a mono-constituent BAC with alkyl-chain length of 12 and high structural similarity to NBD-DDA. Characteristic time-kill kinetics and increased tolerance of a BAC tolerant E. coli strain against NBD-DDA suggest that the mode of action of NBD-DDA is similar to that of BAC. As revealed by confocal laser scanning microscopy (CLSM), NBD-DDA is preferentially localized to the cell envelope of E. coli, which is a primary target of BAC and other QACs. Leveraging these findings and NBD-DDA‘s fluorescent properties, we show that reduced cellular accumulation is responsible for the evolved BAC tolerance in the BAC tolerant E. coli strain and that NBD-DDA is subject to efflux mediated by TolC. Overall, NBD-DDA’s antimicrobial activity, its fluorescent properties, and its ease of detection render it a powerful tool to study resistance mechanisms of QACs in bacteria and highlight its potential to gain detailed insights into its mode-of-action.
KW - Antimicrobial resistance
KW - Bacteria
KW - Disinfection
KW - Biocides
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563811
DO - https://doi.org/10.3389/fmicb.2022.1023326
SN - 1664-302X
IS - 13
SP - 1
EP - 13
PB - Frontiers Media
CY - Lausanne
AN - OPUS4-56381
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rua-Ibarz, Ana
A1 - Nakadi, Flávio V.
A1 - Bolea-Fernandez, Eduardo
A1 - Bazo, Antonio
A1 - Battistella, Beatrice
A1 - Matiushkina, Anna
A1 - Resch-Genger, Ute
A1 - Abad Andrade, Carlos Enrique
A1 - Resano, Martín
T1 - Discrete entity analysis via microwave-induced nitrogen plasma–mass spectrometry in single-event mode
N2 - In this work, single-event microwave-induced nitrogen plasma–mass spectrometry (single-event MINP-MS) was evaluated for the first time for the analysis of discrete entities such as nanoparticles, biological cells, and microplastics. Nitrogen (N2) effectively overcomes Ar-based polyatomic interferences, enabling (ultra)trace element determination of Fe and Se using their most abundant isotopes, 56Fe (91.66%) and 80Se (49.82%). Iron oxide nanoparticles (Fe2O3 NPs) ranging from 20 to 70 nm were accurately characterized, with excellent agreement with established sizing techniques, such as transmission electron microscopy (TEM) and dynamic light scattering (DLS). A limit of detection (LoD) of 8.6 ag for Fe─equivalent to an LoDsize of 19 nm for Fe2O3─was achieved, which is significantly lower than recent values reported for high-end quadrupole-based ICP-MS. Selenium nanoparticles (SeNPs) of 150 and 250 nm were also accurately characterized, without the N2-based plasma experiencing issues handling relatively large metallic NPs (linearity, R2 = 0.9994). Se-enriched yeast cells (SELM-1 certified reference material) were successfully analyzed via single-cell MINP-MS using external calibration based on SeNPs and a transport efficiency-independent approach. In addition, 2–3 μm polystyrene (PS) and polytetrafluoroethylene (PTFE) were accurately sized by monitoring 12C+, confirming the method’s suitability for handling micrometer-sized polymeric materials (microplastics). The average duration of individual events (680 ± 160 μs) suggests that the digestion of individual entities in N2-based plasmas is comparable to that in Ar-based plasmas. These results open new avenues for this instrumentation as an alternative to ICP ionization sources, also in the context of discrete entity analysis.
KW - Microwave-Induced Nitrogen Plasma
KW - Discrete entity analysis
KW - Particle/droplet event counting
KW - Comparison to SP-ICP-MS methodologies
KW - Nitrogen plasma vs. argon ICP trade-offs
KW - Trace elemental quantification at the single-entity level
KW - Time-resolved mass spectrometry for discrete entities
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643825
DO - https://doi.org/10.1021/acs.analchem.5c04341
SN - 0003-2700
SP - 1
EP - 8
PB - American Chemical Society (ACS)
AN - OPUS4-64382
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Morcillo, Dalia
A1 - Winckelmann, Alexander
A1 - Oelze, Marcus
A1 - Leonhardt, Robert
A1 - Schmidt, Anita
A1 - Richter, Silke
A1 - Recknagel, Sebastian
A1 - Vogl, Jochen
A1 - Panne, Ulrich
A1 - Abad Andrade, Carlos Enrique
T1 - Exploring Age-Induced Lithium Isotope Fractionation in Lithium-Ion Batteries using Microwave-Induced Cold Nitrogen Plasma Mass Spectrometry
N2 - This study explores Microwave-Inductively Coupled Atmospheric-pressure Plasma Mass Spectrometry (MICAP-MS) as a cost-effective alternative to Multi-Collector Inductively Coupled Plasma Mass Spectrometry (MC-ICP-MS) for analyzing lithium isotopic composition in lithium-ion batteries (LIBs). We investigate the performance of MICAP-MS in measuring Li isotope ratios in new and aged commercial lithium cobalt oxide (LCO) batteries. Our results show that MICAP-MS, operating under cold plasma conditions at 800 W with an 8 mm torch position, achieves results metrologically compatible with MC-ICP-MS, with a precision ranging from 0.6‰ to 3.4‰ for δ7Li values. MICAP-MS benefits from a dielectric resonator for uniform plasma, better ion velocity control, and higher energy efficiency. Optimal settings were identified with dwell times of 10 ms for 6Li and 1 ms for 7Li. The study of LIBs revealed that 6Li migrates towards the anode over multiple charge–discharge cycles, causing 7Li to accumulate in the cathode, a fractionation effect that becomes more pronounced with prolonged cycling. MICAP-MS provides a cost-effective, precise alternative to MC-ICP-MS, with lower operational costs and enhanced portability, advancing the study of isotopic fractionation and aging in lithium-ion batteries.
KW - MICAP-MS
KW - Lithium
KW - Battery aging
KW - Lithium isotopes
KW - Nitrogen plasma
KW - Isotope fractionation
KW - lithium cobalt oxide
KW - LCO
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643777
DO - https://doi.org/10.1039/d4ja00324a
SN - 0267-9477
SP - 1
EP - 11
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64377
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Abad Andrade, Carlos Enrique
A1 - Jegielka, Dennis
A1 - Aloysius, Allen
A1 - Recknagel, Sebastian
T1 - SI-traceable total analysis of nitrate and nitrite by isotope dilution optical spectroscopy and its application to Berlin surface waters
N2 - Accurate nitrate and nitrite data support water-quality regulation, yet routine methods rely on external calibration and rarely achieve SI traceability. We report a calibration-free determination of nitrate and nitrite by combining isotope dilution with high-resolution continuum-source graphite furnace molecular absorption spectrometry (ID-HR-CS-GF-MAS). A 15N-enriched nitrate spike (its concentration verified by reverse isotope dilution against the standard reference material NIST 3185) provides the SI link, and it is gravimetrically added to samples; nitrate and residual nitrite are converted in situ to nitric oxide (NO), whose 215 nm band is recorded at a pixel resolution of λ/Δλ ≈ 140 000. The 0.2127 nm shift between 14NO and 15NO electronic spectra is resolved, and a three-latent-variable partial least squares regression model yields the 15N/14N ratio with 0.3% precision. Instrumental LoD values of 4.8 ng (14N) and 3.2 ng (15N) translate to a method LoD of 4.8 ng of nitrogen (equivalent to 1.05 mg L−1 NO3− for a 20 μL aliquot). The furnace program allows for successive drying/pyrolysis loops, so additional 20 μL aliquots can be layered onto the graphite platform. Alternatively, a 10 mL anion-exchange solid-phase extraction step concentrates nitrate and nitrite fivefold, allowing for the analysis of even lower sample concentrations. Results for four certified reference materials (2.9 to 1000 mg L−1 NO3−) agreed with certified values, giving relative expanded uncertainties of 2 to 4%. Analysis of twenty Berlin surface-water samples revealed concentrations ranging from 0.10 to 7.3 mg L−1 NO3−, indicating that the Panke River and Teltow Canal are the primary sources of nitrogen. ID-HR-CS-GF-MAS thus delivers ID-MS-level accuracy in a few minutes per run with bench-top optics, and, with optional on-platform or SPE pre-concentration, extends SI-traceable nitrate/nitrite monitoring into the low-ng regime.
KW - Isotope dilution
KW - Nitrate and nitrite determination
KW - SI-traceable quantification
KW - Calibration-free analysis
KW - Water quality
KW - Berlin surface waters
KW - NO molecular absorption bands
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643785
DO - https://doi.org/10.1039/D5JA00252D
SN - 0267-9477
VL - 40
IS - 10
SP - 2692
EP - 2701
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64378
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Klinge, A
A1 - Mönig, J
A1 - Ziegert, C
A1 - Richter, Matthias
A1 - Kalbe, Ute
A1 - Horn, Wolfgang
A1 - Röhlen, U
A1 - Rauscher, S
A1 - Roswag-Klinge, E
T1 - upMIN 100 – upcycling of mineral construction and demolition waste to substitute natural aggregates in earthen building materials
N2 - The construction sector is one of the most resource-intensive sectors in Germany and is responsible for 40 % of CO2 emissions. Around 517 million tons of mineral raw materials are required annually for the construction of buildings in Germany. At the same time, mineral construction waste was the largest material flow at 229.3 million tons (2020). The rates of construction and demolition waste (CDW) recycling have increased since 2000, especially for mineral waste. Nevertheless, the majority of recycled aggregates are used in technically largely unregulated applications (e.g. road construction). This downcycling leads to a loss of valuable resources for technically and economically valuable applications. The upMIN 100 research project is investigating the question of whether and to what extent recycled CDW is suitable as an additive an binder in earthen building materials. The focus is placed on grain sizes of < 2 mm, which are currently predominantly landfilled, as there are at present no regulations for their use in building products. The soil matrix of earthen building materials however, naturally contains of different grain sizes, whith < 2mm – 0,063 for aggregates and < 0.063 mm as a binder. Therefore, the focused grain sizes (sand, clay and silt) could have a high usage potential. In order to enable the use of CDW, the technical feasibility must be ensured, quality requirements for source materials (e.g. threshold values for pollutants in terms of health and environmental compatibility and hazardous substances) and permissible proportions of recycled aggregates must be defined. Two different building material developments (earth blocks and -plaster)were used to assess both, the technical feasibility as well the pollutant content of the recycled aggregate and its final emissions into the indoor air. For both materials two mixtures could be established, that also meet the mechanical specifications according to the DIN standard, such as the compressive strength. A method was developed to design material mixtures with a high amount of CDW that comply with the defined limit values. The mixtures reached a recycling rate of 28 % with high mechanical properties and 70 % with minimum strength requirements.
KW - Mineral waste
KW - Upcycling
KW - Earthen building product
KW - Circular construction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652831
DO - https://doi.org/10.1088/1755-1315/1554/1/012084
SN - 1755-1307
VL - 1554
IS - 1
SP - 1
EP - 9
PB - IOP Publishing
AN - OPUS4-65283
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tavernaro, Isabella
A1 - Rajotte, Isabelle
A1 - Thibeault, Marie-Pier
A1 - Sander, Philipp C.
A1 - Kodra, Oltion
A1 - Lopinski, Gregory
A1 - Radnik, Jörg
A1 - Johnston, Linda J.
A1 - Brinkmann, Andreas
A1 - Resch-Genger, Ute
T1 - Quantifying surface groups on aminated silica nanoparticles of different size, surface chemistry, and porosity with solution NMR, XPS, optical assays, and potentiometric titration
N2 - We assessed the quantification of surface amino functional groups (FGs) for a large set of commercial and custom-made aminated silica nanoparticles (SiO2 NPs) with sizes of 20–100 nm, prepared with different sol–gel routes, different amounts of surface amino FGs, and different porosity with four methods providing different, yet connected measurands in a bilateral study of two laboratories, BAM and NRC, with the overall aim to develop standardizable measurements for surface FG quantification. Special emphasis was dedicated to traceable quantitative magnetic resonance spectroscopy (qNMR) performed with dissolved SiO2 NPs. For the cost efficient and automatable screening of the amount of surface amino FGs done in a first step of this study, the optical fluorescamine assay and a potentiometric titration method were utilized by one partner, i.e., BAM, yielding the amount of primary amino FGs accessible for the reaction with a dye precursor and the total amount of (de)protonatable FGs. These measurements, which give estimates of the minimum and maximum number of surface amino FGs, laid the basis for quantifying the amount of amino silane molecules with chemo-selective qNMR with stepwise fine-tuned workflows, involving centrifugation, drying, weighting, dissolution, measurement, and data evaluation steps jointly performed by BAM and NRC. Data comparability and relative standard deviations (RSDs) obtained by both labs were used as quality measures for method optimization and as prerequisites to identify method-inherent limitations to be later considered for standardized measurement protocols. Additionally, the nitrogen (N) to silicon (Si) ratio in the near-surface region of the SiO2 NPs was determined by both labs using X-ray photoelectron spectroscopy (XPS), a well established surface sensitive analytical method increasingly utilized for microparticles and nano-objects which is currently also in the focus of international standardization activities. Overall, our results underline the importance of multi-method characterization studies for quantifying FGs on NMs involving at least two expert laboratories for effectively identifying sources of uncertainty, validating analytical methods, and deriving NM structure–property relationships.
KW - Advanced Materials
KW - Amino Groups
KW - Calibration
KW - Characterization
KW - Functional groups
KW - Method Comparison
KW - Nano Particle
KW - Validation
KW - XPS
KW - Optical Assay
KW - Quantification
KW - Surface Analysis
KW - Reference Materials
KW - Synthesis
KW - Fluorescence
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649992
DO - https://doi.org/10.1039/d5na00794a
VL - 7
IS - 21
SP - 6888
EP - 6900
PB - Royal Society of Chemistry
AN - OPUS4-64999
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schusterbauer, Robert
A1 - Schünemann, Pia
A1 - Nickl, Philip
A1 - Er, Jasmin
A1 - Kämmer, Victoria
A1 - Junge, Florian
A1 - Fazzani, Salim
A1 - Mrkwitschka, Paul
A1 - Meermann, Björn
A1 - Haag, Rainer
A1 - Donskyi, Ievgen
T1 - Bifunctional Reduced Graphene Oxide Derivatives for PFOA Adsorption
N2 - Innovative materials are crucial for removing persistent pollutants per‐ and polyfluorinated alkyl substances (PFAS) from water. Here, a novel bifunctional reduced graphene oxide (TRGO) adsorbent is developed and characterized by advanced surface sensitive methods. Compared to pristine TRGO, the functionalized TRGO shows markedly improved PFAS removal efficiency and demonstrates strong potential for water purification applications.
KW - Adsorber
KW - PFAS
KW - HR-CS-GFMAS
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651238
DO - https://doi.org/10.1002/ceur.202500240
SN - 2751-4765
SP - 1
EP - 7
PB - Wiley VHC-Verlag
AN - OPUS4-65123
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kazlagić, Anera
A1 - Vogl, Jochen
A1 - Gluth, Gregor
A1 - Stephan, D.
T1 - Provenancing of cement using elemental analyses and isotope techniques – The state-of-the-art and future perspectives
N2 - With the aim of identifying the origin and the manufacturer of a cement, a reliable procedure that provides unambiguous results is needed. Such procedure could resolve practical issues in damage research, liability issues and forensic investigations. A substantial number of attempts for fingerprinting of building materials, including cement, has already been carried out during the last decades. Most of them were based on concentration analysis of the main elements/components. This review provides an overview of provenance studies of cement and the main approaches commonly used. Provenance studies of cement via isotope techniques are also presented and discussed as representatives of the state-of-the-art in the field. Due to the characteristic properties and the occurrence of carefully selected isotope ratios, unique fingerprints of different kinds of materials can be provided by these methods. This property has largely been explored in various scientific fields such as geo- and cosmochemistry, food forensics, archaeology, geochronology, biomedical studies, and climate change processes. However, the potential of isotope techniques in cement and concrete research for provenance studies has barely been investigated.
Therefore, the review outlines a suitable approach using isotope ratios, which could lead to reliable provenancing of cementitious materials in the future.
KW - Cement
KW - Sr isotopes
KW - Provenance
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533762
DO - https://doi.org/10.1039/d1ja00144b
VL - 36
IS - 10
SP - 2030
EP - 2042
PB - The Royal Society of Chemistry
CY - Cambridge, UK
AN - OPUS4-53376
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Weigert, Florian
A1 - Müller, A.
A1 - Häusler, I.
A1 - Geißler, Daniel
A1 - Skroblin, D.
A1 - Unger, Wolfgang
A1 - Radnik, Jörg
A1 - Resch-Genger, Ute
T1 - Combining HR‑TEM and XPS to elucidate the core–shell structure of ultrabright CdSe/CdS semiconductor quantum dots
N2 - Controlling thickness and tightness of surface passivation shells is crucial for many applications of core–shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the applicationrelevant functionality like a high photoluminescence (PL) quantum yield, calling for a whole nanoobject approach. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. In addition to demonstrating the potential of this novel whole nanoobject approach for determining architectures of small nanoparticles, the presented results also highlight challenges faced by different sizing and structural analysis methods and method-inherent uncertainties.
KW - Photoluminescence
KW - Single particle
KW - Microscopy
KW - Particle architecture
KW - Thickness
KW - SAXS
KW - Shell
KW - XPS
KW - TEM
KW - Semiconductor
KW - Quantum dot
KW - Photophysics
KW - Quantum yield
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517911
DO - https://doi.org/10.1038/s41598-020-77530-z
VL - 10
IS - 1
SP - 20712
PB - Springer Nature
AN - OPUS4-51791
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Radnik, Jörg
A1 - Knigge, Xenia
A1 - Andresen, Elina
A1 - Resch-Genger, Ute
A1 - Cant, D.J.H.
A1 - Shard, A.G.
A1 - Clifford, C.A.
T1 - Composition, thickness, and homogeneity of the coating of core–shell nanoparticles—possibilities, limits, and challenges of X-ray photoelectron spectroscopy
N2 - Core–shell nanoparticles have attracted much attention in recent years due to their unique properties and their increasing importance in many technological and consumer products. However, the chemistry of nanoparticles is still rarely investigated in comparison to their size and morphology. In this review, the possibilities, limits, and challenges of X-ray photoelectron spectroscopy (XPS) for obtaining more insights into the composition, thickness, and homogeneity of nanoparticle coatings are discussed with four examples: CdSe/CdS quantum dots with a thick coating and a small core; NaYF4-based upconverting nanoparticles with a large Yb-doped core and a thin Er-doped coating; and two types of polymer nanoparticles with a poly(tetrafluoroethylene) core with either a poly(methyl methacrylate) or polystyrene coating. Different approaches for calculating the thickness of the coating are presented, like a simple numerical modelling or a more complex simulation of the photoelectron peaks. Additionally, modelling of the XPS background for the investigation of coating is discussed. Furthermore, the new possibilities to measure with varying excitation energies or with hard-energy X-ray sources (hard-energy X-ray photoelectron spectroscopy) are described. A discussion about the sources of uncertainty for the determination of the thickness of the coating completes this review.
KW - X-ray spectroscopy
KW - Nanoparticles
KW - Spectroscopy / Instrumentation
KW - Spectroscopy / Theory
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548305
DO - https://doi.org/10.1007/s00216-022-04057-9
VL - 414
IS - 15
SP - 4331
EP - 4345
PB - SpringerNature
AN - OPUS4-54830
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Junge, Florian
A1 - Wittwer, Philipp
A1 - Sommerfeld, Thomas
A1 - Gehrenkemper, Lennart
A1 - Zoister, Christian
A1 - Nickl, Philip
A1 - Koch, Matthias
A1 - Meermann, Björn
A1 - Haag, Rainer
T1 - Adsorber Charge Dominates over Hydrophobic or Fluorophilic Functionalization in Influencing Adsorption of PFCA onto Polystyrene Resins
N2 - A systematic series of industrial-relevant polystyrene-based anion exchange resins that are functionalized with hydro- or fluorocarbon chains are compared regarding their adsorption behavior toward perfluorocarboxylic acids (PFCA) in respect to their charge, chain length, and type of chain. The results clearly show the dominance of electrostatic interactions in the adsorption process as uncharged adsorber materials showed no adsorption at all. In contrast, the charged adsorber materials showed in general a PFCA removal of 80% to 30% over the experiment depending on effluent fraction.
Unexpectedly, for perfluorobutanoic acid (PFBA) the highest removal rate is found with consistently >90%. Despite observing significant benefits in the adsorption of PFCA for fluoroalkylated adsorbers in comparison to their non-fluorinated counterparts, this effect of fluoroalkylation is comparatively small and can not be clearly attributed to fluorophilic interactions between the fluoroalkyl chains. These findings help clarifying that the introduction of fluorocarbon moieties in adsorber materials is not necessary in order to remove fluorocarbon molecules from the environment.
KW - PFAS
KW - Remediation
KW - Adsorption
KW - Fluorophilic interactions
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601883
DO - https://doi.org/10.1002/admi.202400199
SN - 2196-7350
SP - 1
EP - 10
PB - John Wiley & Sons
CY - Hoboken, New Jersey, USA
AN - OPUS4-60188
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mangarova, Dilyana B.
A1 - Kaufmann, Jan Ole
A1 - Brangsch, Julia
A1 - Kader, Avan
A1 - Möckel, Jana
A1 - Heyl, Jennifer L.
A1 - Verlemann, Christine
A1 - Adams, Lisa C.
A1 - Ludwig, Antje
A1 - Reimann, Carolin
A1 - Poller, Wolfram C.
A1 - Niehaus, Peter
A1 - Karst, Uwe
A1 - Taupitz, Matthias
A1 - Hamm, Bernd
A1 - Weller, Michael G.
A1 - Makowski, Marcus R.
T1 - ADAMTS4-Specific MR Peptide Probe for the Assessment of Atherosclerotic Plaque Burden in a Mouse Model
N2 - Introduction
Atherosclerosis is the underlying cause of multiple cardiovascular pathologies. The present-day clinical imaging modalities do not offer sufficient information on plaque composition or rupture risk. A disintegrin and metalloproteinase with thrombospondin motifs 4 (ADAMTS4) is a strongly upregulated proteoglycan-cleaving enzyme that is specific to cardiovascular diseases, inter alia, atherosclerosis.
Materials and Methods
Male apolipoprotein E-deficient mice received a high-fat diet for 2 (n = 11) or 4 months (n = 11). Additionally, a group (n = 11) receiving pravastatin by drinking water for 4 months alongside the high-fat diet was examined. The control group (n = 10) consisted of C57BL/6J mice on standard chow. Molecular magnetic resonance imaging was performed prior to and after administration of the gadolinium (Gd)-based ADAMTS4-specific probe, followed by ex vivo analyses of the aortic arch, brachiocephalic arteries, and carotid arteries. A P value <0.05 was considered to indicate a statistically significant difference.
Results
With advancing atherosclerosis, a significant increase in the contrast-to-noise ratio was measured after intravenous application of the probe (mean precontrast = 2.25; mean postcontrast = 11.47, P < 0.001 in the 4-month group). The pravastatin group presented decreased ADAMTS4 expression. A strong correlation between ADAMTS4 content measured via immunofluorescence staining and an increase in the contrast-to-noise ratio was detected (R2 = 0.69). Microdissection analysis revealed that ADAMTS4 gene expression in the plaque area was significantly greater than that in the arterial wall of a control mouse (P < 0.001). Laser ablation–inductively coupled plasma–mass spectrometry confirmed strong colocalization of areas positive for ADAMTS4 and Gd.
Conclusions
Magnetic resonance imaging using an ADAMTS4-specific agent is a promising method for characterizing atherosclerotic plaques and could improve plaque assessment in the diagnosis and treatment of atherosclerosis.
N2 - Einleitung
Atherosklerose ist die Ursache für zahlreiche Herz-Kreislauf-Erkrankungen. Die derzeitigen klinischen Bildgebungsverfahren liefern keine ausreichenden Informationen über die Zusammensetzung von Plaques oder das Risiko einer Ruptur. A Disintegrin and Metalloproteinase with Thrombospondin Motifs 4 (ADAMTS4) ist ein stark hochreguliertes Proteoglykan-spaltendes Enzym, das unter anderem bei Herz-Kreislauf-Erkrankungen wie Atherosklerose spezifisch auftritt.
Materialien und Methoden
Männliche Apolipoprotein-E-defiziente Mäuse erhielten 2 (n = 11) oder 4 Monate lang (n = 11) eine fettreiche Ernährung. Zusätzlich wurde eine Gruppe (n = 11) untersucht, die 4 Monate lang neben der fettreichen Ernährung Pravastatin über das Trinkwasser erhielt. Die Kontrollgruppe (n = 10) bestand aus C57BL/6J-Mäusen, die mit Standardfutter ernährt wurden. Vor und nach der Verabreichung der gadolinium (Gd)-basierten ADAMTS4-spezifischen Sonde wurde eine molekulare Magnetresonanztomographie durchgeführt, gefolgt von Ex-vivo-Analysen des Aortenbogens, der Arteria brachiocephalica und der Arteria carotis. Ein P-Wert < 0,05 wurde als statistisch signifikanter Unterschied gewertet.
Ergebnisse
Mit fortschreitender Atherosklerose wurde nach intravenöser Anwendung der Sonde ein signifikanter Anstieg des Kontrast-Rausch-Verhältnisses gemessen (Mittelwert vor Kontrastmittelgabe = 2,25; Mittelwert nach Kontrastmittelgabe = 11,47, P < 0,001 in der 4-Monats-Gruppe). Die Pravastatin-Gruppe zeigte eine verminderte ADAMTS4-Expression. Es wurde eine starke Korrelation zwischen dem mittels Immunfluoreszenzfärbung gemessenen ADAMTS4-Gehalt und einem Anstieg des Kontrast-Rausch-Verhältnisses festgestellt (R2 = 0,69). Die Mikrodissektionsanalyse ergab, dass die ADAMTS4-Genexpression im Plaque-Bereich signifikant höher war als in der Arterienwand einer Kontrollmaus (P < 0,001). Laserablation-induktiv gekoppelte Plasma-Massenspektrometrie bestätigte eine starke Kolokalisierung von ADAMTS4- und Gd-positiven Bereichen.
Schlussfolgerungen
Die Magnetresonanztomographie mit einem ADAMTS4-spezifischen Kontrastmittel ist eine vielversprechende Methode zur Charakterisierung atherosklerotischer Plaques und könnte die Plaquebewertung in der Diagnose und Behandlung von Atherosklerose verbessern.
KW - Peptide Aptamer
KW - MRI Probe
KW - Magnetic resonance imaging (MRI)
KW - Peptide libraries
KW - Laser ablation–inductively coupled plasma–mass spectrometry
KW - ICP MS
KW - Imaging
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635832
DO - https://doi.org/10.1097/RLI.0000000000001152
SN - 1536-0210
VL - 60
IS - 8
SP - 499
EP - 507
PB - Ovid Technologies (Wolters Kluwer Health)
CY - Philadelphia, Pennsylvania, USA
AN - OPUS4-63583
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Döring, Sarah
A1 - Konthur, Zoltán
A1 - Weller, Michael G.
A1 - Jaeger, Carsten
A1 - Reinders, Yvonne
T1 - Challenges and Insights in Absolute Quantification of Recombinant Therapeutic Antibodies by Mass Spectrometry: An Introductory Review
N2 - This review describes mass spectrometry (MS)-based approaches for the absolute quantification of therapeutic monoclonal antibodies (mAbs), focusing on technical challenges in sample treatment and calibration. Therapeutic mAbs are crucial for treating cancer and inflammatory, infectious, and autoimmune diseases. We trace their development from hybridoma technology and the first murine mAbs in 1975 to today’s chimeric and fully human mAbs. With increasing commercial relevance, the absolute quantification of mAbs, traceable to an international standard system of units (SI units), has attracted attention from science, industry, and national metrology institutes (NMIs). Quantification of proteotypic peptides after enzymatic digestion using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has emerged as the most viable strategy, though methods targeting intact mAbs are still being explored. We review peptide-based quantification, focusing on critical experimental steps like denaturation, reduction, alkylation, choice of digestion enzyme, and selection of signature peptides. Challenges in amino acid analysis (AAA) for quantifying pure mAbs and peptide calibrators, along with software tools for targeted MS data analysis, are also discussed. Short explanations within each chapter provide newcomers with an overview of the field’s challenges. We conclude that, despite recent progress, further efforts are needed to overcome the many technical hurdles along the quantification workflow and discuss the prospects of developing standardized protocols and certified reference materials (CRMs) for this goal. We also suggest future applications of newer technologies for absolute mAb quantification.
KW - Monoclonal antibody
KW - Therapeutic antibodies
KW - Mass spectrometry
KW - Liquid chromatography
KW - Absolute quantification
KW - Metrology
KW - Traceability
KW - Certified reference material
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623707
DO - https://doi.org/10.3390/antib14010003
SN - 2073-4468
VL - 14
IS - 1
SP - 1
EP - 26
PB - MDPI
CY - Basel, Schweiz
AN - OPUS4-62370
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - 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 - Bhattacharya, Biswajit
A1 - Michalchuk, Adam
A1 - Silbernagl, Dorothee
A1 - Rautenberg, Max
A1 - Schmid, Thomas
A1 - Feiler, Torvid
A1 - Reimann, K.
A1 - Ghalgaoui, A.
A1 - Sturm, Heinz
A1 - Paulus, B.
A1 - Emmerling, Franziska
T1 - A Mechanistic Perspective on Plastically Flexible Coordination Polymers
N2 - Mechanical flexibility in single crystals of covalently bound materials is a fascinating and poorly understood phenomenon. We present here the first example of a plastically flexible one-dimensional (1D) coordination polymer. The compound [Zn(m-Cl)2(3,5-dichloropyridine)2]n is flexible over two crystallographic faces. Remarkably, the single crystal remains intact when bent to 1808. A combination of microscopy, diffraction, and spectroscopic studies have been used to probe the structural response of the crystal lattice to mechanical bending. Deformation of the covalent polymer chains does not appear to be responsible for the observed macroscopic bending. Instead, our results suggest that mechanical bending occurs by displacement of the coordination polymer chains. Based on experimental and theoretical evidence, we propose a new model for mechanical flexibility in 1D coordination polymers. Moreover, our calculations propose a cause of the different mechanical properties of this compound and a structurally similar elastic material
KW - Coordination polymer
KW - Flexible crystals
KW - Mechanical properties
KW - Plastic deformation
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504755
DO - https://doi.org/10.1002/anie.201914798
VL - 59
IS - 14
SP - 5557
EP - 5561
PB - Wiley-VCH
AN - OPUS4-50475
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Martins, Ines
A1 - Al-Sabbagh, Dominik
A1 - Bentrup, U.
A1 - Marquardt, Julien
A1 - Schmid, Thomas
A1 - Scoppola, E.
A1 - Kraus, Werner
A1 - Stawski, Tomasz
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Yusenko, Kirill
A1 - Weidner, Steffen
A1 - Emmerling, Franziska
T1 - Formation Mechanism of a Nano-Ring of Bismuth Cations and Mono-Lacunary Keggin-Type Phosphomolybdate
N2 - A new hetero-bimetallic polyoxometalate (POM) nano-ring was synthesized in a one-pot procedure. The structure consists of tetrameric units containing four bismuth-substituted monolacunary Keggin anions including distorted [BiO8] cubes. The nano-ring is formed via self-assembly from metal precursors in aqueous acidic medium. The compound (NH4)16[(BiPMo11O39)4] ⋅ 22 H2O; (P4Bi4Mo44) was characterized by single-crystal X-ray diffraction, extended X-ray absorption fine structure spectroscopy (EXAFS), Raman spectroscopy, matrix-assisted laser desorption/ionisation-time of flight mass spectrometry (MALDI-TOF), and thermogravimetry/differential scanning calorimetry mass spectrometry (TG-DSC-MS). The formation of the nano-ring in solution was studied by time-resolved in situ small- and wide-angle X-ray scattering (SAXS/WAXS) and in situ EXAFS measurements at the Mo−K and the Bi−L3 edge indicating a two-step process consisting of condensation of Mo-anions and formation of Bi−Mo-units followed by a rapid self-assembly to yield the final tetrameric ring structure.
KW - Bismuth
KW - In situ EXAFS
KW - In situ SAXS/WAXS
KW - Lacunary Keggin ion
KW - Polyoxometalates
KW - Self-assembly
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546823
DO - https://doi.org/10.1002/chem.202200079
SN - 0947-6539
VL - 28
IS - 27
SP - 1
EP - 7
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-54682
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zänker, Steffen
A1 - Scholz, G.
A1 - Marquardt, Julien
A1 - Emmerling, Franziska
T1 - Structural changes in Ba-compounds of different hardness induced by high-energy ball milling – evidenced by 137Ba NMR and X-ray powder diffraction
N2 - Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors.
KW - Mechanochemistry
KW - X-ray diffraction
KW - Solid state NMR
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547397
DO - https://doi.org/10.1002/zaac.202200026
SN - 0044-2313
VL - 648
IS - 10
SP - 1
EP - 8
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-54739
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gugin, Nikita
A1 - Villajos Collado, José Antonio
A1 - Feldmann, Ines
A1 - Emmerling, Franziska
T1 - Mix and wait – a relaxed way for synthesizing ZIF-8
N2 - Herein we report the synthesis of a zeolitic imidazolate framework (ZIF-8) by an easy “mix and wait” procedure. In a closed vial, without any interference, the mixture of 2-methylimidazole and basic zinc carbonate assembles into the crystalline product with approx. 90% conversion after 70 h. The reaction exhibits sigmoidal kinetics due to the self-generated water which accelerates the reaction.
KW - In-situ analysis
KW - Mechanochemistry
KW - MOF
KW - Synthesis
KW - ZIF-8
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546841
DO - https://doi.org/10.1039/D2RA00740A
VL - 12
SP - 8940
EP - 8944
PB - Royal Society of Chemistry
AN - OPUS4-54684
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -