TY - JOUR
A1 - You, Yi
A1 - Xue, Boyang
A1 - Riedel, Jens
T1 - Enhancement of LIBS plasma in air with organic solvent vapors
N2 - Laser-induced breakdown spectroscopy (LIBS) offers versatile, field-deployable elemental analysis; however, compact, high-repetition-rate nanosecond laser systems typically face constraints in power consumption and size, often compromising emission intensity and thus analytical performance. We demonstrate a significant improvement in LIBS signals through the controlled introduction of common organic solvent vapors into a sheath gas, with a diode-pumped solid-state laser (1064 nm, 2–28 kHz repetition rate, 450–600-μJ pulse energy). Optical and acoustic diagnostics reveal up to ca. 40-fold enhancement of the N II emission line at 567 nm when ambient air serves as the analyte. Maximal enhancement occurs at intermediate repetition rates of ca. 15 kHz, particularly at pulse energies approaching the optical breakdown threshold; this observation suggests a viable strategy for operating LIBS at lower pulse energies and higher repetition rates. Enhancement effects scale jointly with both vapor pressure and ionization energy of the organic species, with acetone and toluene markedly outperforming methanol and isopropanol. These findings provide a rational foundation for significantly improving the analytical performance of portable LIBS instruments without exceeding platform-specific constraints.
KW - LIBS
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653758
DO - https://doi.org/10.1016/j.sab.2025.107309
SN - 0584-8547
VL - 236
SP - 1
EP - 6
PB - Elsevier B.V.
AN - OPUS4-65375
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodriguez, Santiago
A1 - Kumanski, Sylvain
A1 - Ayed, Zeineb
A1 - Fournet, Aurélie
A1 - Bouanchaud, Charlène
A1 - Sagar, Amin
A1 - Allemand, Frédéric
A1 - Baulin, Vladimir A.
A1 - Resch‐Genger, Ute
A1 - Cortés, Juan
A1 - Sibille, Nathalie
A1 - Chirot, Fabien
A1 - Wegner, Karl David
A1 - Antoine, Rodolphe
A1 - Le Guével, Xavier
A1 - Bernadó, Pau
T1 - Programming the Optoelectronic Properties of Atomically Precise Gold Nanoclusters Using the Conformational Landscape of Intrinsically Disordered Proteins
N2 - The rational design of hybrid nanomaterials with precisely controlled properties remains a central challenge in materials science. While atomically precise gold nanoclusters (Au‐NCs) offer molecule‐like control over a metallic core, tuning their optoelectronic behavior via surface engineering is often empirically driven. Here, we establish a design principle by demonstrating that the conformational landscape of intrinsically disordered proteins (IDP) can be used as a programmable scaffold to rationally modulate the photophysical properties of a covalently bound Au‐NC. We synthesized a series of bioconjugates between Au 25 nanoclusters and bioengineered IDPs containing a variable number of cysteine anchoring points. A combination of mass spectrometry, small‐angle X‐ray scattering, and modeling on the conjugates indicates that increasing the number of covalent anchors systematically restricts the conformational ensemble, inducing a progressively more compact protein shell around nanoclusters. This structural rigidification at the interface directly translates into a 15‐fold enhancement of the Au‐NC near‐infrared photoluminescence and a six‐fold increase in its average lifetime. Our findings demonstrate that the conformational plasticity of IDPs and the capacity to engineer them can be harnessed as a molecular tuning knob, moving to a new regime of programmable soft‐matter control over the properties of quantum‐confined nanomaterials for tailored biotechnological applications.
KW - Fluorescence
KW - Custer
KW - Nano
KW - Advanced material
KW - Characterization
KW - Fluorescence quantum yield
KW - Integrating sphere spectroscopy
KW - Thiol ligands
KW - Gold
KW - Surface chemistry
KW - SWIR
KW - Mass spectrometry
KW - Protein
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655086
DO - https://doi.org/10.1002/chem.202502991
SN - 0947-6539
SP - 1
EP - 9
PB - Wiley VHC-Verlag
AN - OPUS4-65508
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 - 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 - 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 - 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 - Scholl, Juliane
A1 - Scharpmann, Philippa
A1 - Bagheri, Abbas
A1 - Lisec, Jan
A1 - Meiers, Emelie
A1 - Jaeger, Carsten
A1 - Leonhardt, Robert
A1 - Haase, Hajo
A1 - Koch, Matthias
T1 - Beyond the lab: Real-world composition of commercial Li-ion battery electrolytes
N2 - This study presents a systematic, characterization of electrolytes from commercial lithium-ion batteries (LIB), encompassing 90 batteries from leading global manufacturers across diverse formats and application sectors. An integrated, complementary mass spectrometric workflow combining LC–MS/MS, GC–MS, and high-resolution MS was employed. To ensure robust structural annotation, molecular identifications were assigned confidence levels following Schymanski et al. (2014).
Across all formats, PF6− was confirmed as the dominant Li+ counterion, frequently coexisting with BF4−, PO2F2−, and bis(fluorosulfonyl)imide (FSI−), forming binary and ternary salt systems optimized for both conductivity and safety. Solvent systems revealed the widespread use of propylene carbonate (PC) combined with diverse carbonate mixtures, demonstrating trends in performance optimization specific to cell format. A variety of additives were identified, reflecting a clear shift towards multifunctional, synergistic additive packages and the gradual replacement of fluorinated species with environmentally safer alternatives. Cycling studies demonstrated that electrolyte degradation mechanisms are strongly influenced by electrode composition and additive chemistry, with oxidative degradation pathways dominating.
Together, these findings provide rare empirical insight into the evolving formulation strategies of electrolytes in commercial LIB, still employing classic carbonates and LiPF6, but highlighting a trend toward safer, more robust, and sustainable electrolyte architectures by using synergistic multifunctional systems.
KW - Mass Spectrometry
KW - Lithium-ion batteries
KW - Electrolyte degradation
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656254
DO - https://doi.org/10.1016/j.jpowsour.2026.239739
SN - 0378-7753
VL - 673
SP - 1
EP - 13
PB - Elsevier B.V.
AN - OPUS4-65625
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gugin, Nikita
A1 - Schwab, Alexander
A1 - Carraro, Francesco
A1 - Tavernaro, Isabella
A1 - Falkenhagen, Jana
A1 - Villajos, Jose
A1 - Falcaro, Paolo
A1 - Emmerling, Franziska
T1 - ZIF-8-based biocomposites via reactive extrusion: towards industrial-scale manufacturing
N2 - Mechanochemistry, a sustainable synthetic method that minimizes solvent use, has shown great promise in producing metal–organic framework (MOF)-based biocomposites through ball milling. While ball milling offers fast reaction times, biocompatible conditions, and access to previously unattainable biocomposites, it is a batch-type process typically limited to gram-scale production, which is insufficient to meet commercial capacity. We introduce a scalable approach for the continuous solid-state production of MOF-based biocomposites. Our study commences with model batch reactions to examine the encapsulation of various biomolecules into Zeolitic Imidazolate Framework-8 (ZIF-8) via hand mixing, establishing a foundation for upscaling. Subsequently, the process is scaled up using reactive extrusion, enabling continuous and reproducible kilogram-scale production of bovine serum albumin (BSA)@ZIF-8 with tunable protein loading. Furthermore, we achieve the one-step formation of shaped ZIF-8 extrudates encapsulating clinical therapeutic hyaluronic acid (HA). Upon release of HA from the composite, the molecular weight of HA is preserved, highlighting the industrial potential of reactive extrusion for the cost-effective and reliable manufacturing of biocomposites for drug-delivery applications.
KW - Mechanochemistry
KW - Extrusion
KW - Biocompoites
KW - MOFs
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654777
DO - https://doi.org/10.1039/D5TA08276E
SN - 2050-7496
SP - 1
EP - 14
PB - Royal Society of Chemistry
AN - OPUS4-65477
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tuma, Dirk
A1 - Mady, A. H.
A1 - Baynosa, M. L.
A1 - Saad, M.
A1 - Dhakal, G.
A1 - Kim, W. K.
A1 - Shim, Jae-Jin
T1 - Morphology-engineered hollow NiTiO₃/C–Ag/Ag₃PO₄ S-scheme heterojunction photocatalyst: mechanistic insights into sunlight-driven tetracycline degradation
N2 - Tetracycline (TCH), a widely used antibiotic, persists in aquatic and terrestrial environments, posing ecological risks and accelerating antibiotic resistance. To address this, we report a hollow-structured NiTiO₃/C–Ag/Ag₃PO₄ (NT/C–AAP)
photocatalyst—the first hollow-type nickel titanate—synthesized via a self-template solvothermal route followed by photodeposition. The catalyst integrates key design strategies—hollow architecture, oxygen vacancies, carbon coating, and an S-scheme heterojunction—to optimize photocatalytic performance. The hollow structure enhances light harvesting via internal scattering, oxygen vacancies facilitate O2 adsorption and superoxide (O₂•⁻) generation, and the S-scheme heterojunction effectively suppresses electron–hole recombination while preserving strong redox potential. NT/C–AAP achieved 96% TCH degradation within 1 h and 82% mineralization in 3 h under solar light, far exceeding core–shell (18%) and aggregated (47%) NiTiO₃-based catalysts. Complete removal was realized within 40 min under 400 W visible light. The catalyst maintained 96% activity after five cycles, confirming excellent durability. Compared with previously reported NiTiO₃ photocatalysts, NT/C–AAP delivered a 50–400% performance enhancement arising from its engineered hollow structure and improved electronic properties. Mechanistic studies identified O₂•⁻ and •OH radicals as dominant species, validating the role of morphology and interface engineering in directing charge separation and redox activity. Additionally, a catalyst performance index was proposed to facilitate comparison across diverse conditions. Overall, this work introduces a novel, durable photocatalyst that links structural design to functional performance and demonstrates strong potential for practical environmental remediation.
KW - Heterojunction photocatalyst
KW - Photodegradation
KW - Tetracycline
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655946
DO - https://doi.org/10.1007/s42114-025-01600-x
SN - 2522-0128
VL - 9
IS - 2
SP - 1
EP - 19
PB - Springer Nature
CY - London
AN - OPUS4-65594
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Simon, Fabian
A1 - von der Au, Marcus
A1 - Gehrenkemper, Lennart
A1 - Meermann, Björn
T1 - An optimized method for PFAS analysis using HR–CS–GFMAS via GaF detection
N2 - The analysis of per- and polyfluoroalkyl substances (PFAS) via sum parameters like extractable organic fluorine (EOF) in combination with high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR–CS–GFMAS) is highly promising regarding fluorine sensitivity and selectivity. However, the HR–CS–GFMAS method includes several drying and heating steps which can lead to losses of volatile PFAS before the molecular formation step using e.g., GaF formation. Hence, the method leads to a strong discrimination of PFAS within the EOF depending on their physical/chemical properties and is therefore associated with reduced accuracy. To reduce this discrepancy and to indicate realistic PFAS pollution values, an optimization of the HR–CS–GFMAS method for PFAS analysis is needed. Hence, we determined fluorine response factors of several PFAS with different physical/chemical properties upon application of systematic optimization steps. We could therefore improve the method's sensitivity for PFAS analysis using a modifier drying pre-treatment step followed by a sequential injection of sample solutions. The highest improvement in sensitivity of volatile PFAS was shown upon addition of a Mg modifier during drying pre-treatment. Thereby, during optimization the relative standard deviation of fluorine response factors could be reduced from 55 % (initial method) to 27 % (optimized method) leading to a more accurate determination of organofluorine sum parameters. The method provides an instrumental LOD and LOQ of β(F) 1.71 μg/L and 5.13 μg/L, respectively. Further validation aimed to investigate several matrix effects with respect to water matrices. Here, substance-specific behavior was observed. For example, perfluorooctanoic acid (PFOA) which was used as calibrator, showed signal suppressions upon high chloride concentrations (>50 mg/L). Hence, a thorough separation of Cl from analytes during sample preparation is needed for accurate sum parameter analysis.
KW - PFAS
KW - GF-AAS
KW - Method optimization
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610522
DO - https://doi.org/10.1016/j.talanta.2024.126811
VL - 281
SP - 1
EP - 11
PB - Elsevier B.V.
AN - OPUS4-61052
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zöllner, Moritz T.
A1 - Dariz, Petra
A1 - Riedel, Jens
A1 - Schmid, Thomas
T1 - Dolomite and Mg Calcite as Mineral Thermometers in Mortar Binders. A High Resolution Raman Spectroscopic Study
N2 - This paper suggests the use of high‐resolution Raman scattering bands of MgCa carbonates as posteriori thermometer minerals in archaeometric studies. Therefore, the thermal behavior of two dolomite samples and the hydration and carbonation reaction in air of the decomposition products were investigated by Raman microspectroscopy. The increase in the calcination temperature resulted in the formation of – Raman silent MgO and – inert Mg calcite at 700°C–750°C. In contrast, the decarbonation, hydration, and recarbonation of sample material exposed to 750°C–900°C in a muffle furnace led to the appearance of Mg‐free calcite. High spectral resolution Raman spectroscopy enabled a spectral distinction between these two groups due to differences in the band parameters (peak position, bandwidth) of the vibrational (v1, v4, L) modes of calcite. In combination with Raman microspectroscopic mapping, this spectral information represents a new approach for the estimation of burning temperatures of medieval high‐fired gypsum mortars via natural dolomite impurities. Thus, the results of this work highlight the importance and potential of Raman microspectroscopy as a thermometric tool for elucidating the thermal history of anthropogenic fired materials, with potential applications for archaeometry and art technology, as well as for quality controls in the frame of the production of mineral mortar binders and ceramics or bricks, respectively.
KW - Mineral thermometry
KW - Raman spectroscopy
KW - Dolomite
KW - High-fired gypsum mortar
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630270
DO - https://doi.org/10.1002/jrs.6810
SN - 1097-4555
SP - 1
EP - 13
PB - Wiley
AN - OPUS4-63027
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - McGonigle, Rebecca
A1 - Glasgow, Jodie
A1 - Houston, Catriona
A1 - Cameron, Iain
A1 - Homann, Christian
A1 - Black, Dominic J.
A1 - Pal, Robert
A1 - MacKenzie, Lewis E.
ED - MacKenzie, Lewis E.
T1 - Autoclave reactor synthesis of upconversion nanoparticles, unreported variables, and safety considerations
N2 - Autoclave reactors are widely used across chemical and biological sciences, including for the synthesis of upconversion nanoparticles (UCNPs) and other nanomaterials. Yet, the details of how autoclave reactors are used in such synthesis are rarely reported in the literature, leaving several key synthesis variables widely unreported and thereby hampering experimental reproducibility. In this perspective, we discuss the safety considerations of autoclave reactors and note that autoclaves should only be used if they are (a) purchased from reputable suppliers/manufacturers and (b) have been certified compliant with relevant safety standards. Ultimately, using unsuitable autoclave equipment can pose a severe physical hazard and may breach legal safety requirements. In addition, we highlight several parameters in autoclave synthesis that should be reported as standard to maximise the reproducibility of autoclave synthesis experiments across materials and chemistry research. We encourage users of autoclave synthesis vessels to: (1) adopt high-safety autoclaves and (2) report the many experimental variables involved to enhance experimental reproducibility.
KW - Reference material
KW - Nano
KW - Particle
KW - Shell
KW - Fluorescence
KW - Lifetime
KW - Decay kinetics
KW - Synthesis
KW - Quality assurance
KW - Method
KW - Energy transfer
KW - Upconversion
KW - Autoclave synthesis
KW - Data comparability
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625672
DO - https://doi.org/10.1038/s42004-025-01415-3
VL - 8
IS - 1
SP - 1
EP - 7
PB - Springer Science and Business Media LLC
AN - OPUS4-62567
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Duarte Bernardino, Carolina
A1 - Lee, Mihyun
A1 - Ren, Qun
A1 - Ruehle, Bastian
T1 - Facile Spray-Coating of Antimicrobial Silica Nanoparticles for High-Touch Surface Protection
N2 - The rising threat from infectious pathogens poses an ever-growing challenge. Metal-based nanomaterials have gained a great deal of attention as active components in antimicrobial coatings. Here, we report on the development of readily deployable, sprayable antimicrobial surface coatings for high-touch stainless steel surfaces that are ubiquitous in many healthcare facilities to combat the spread of pathogens. We synthesized mesoporous silica nanoparticles (MSNs) with different surface functional groups, namely, amine (MSN-NH2), carboxy (MSN-COOH), and thiol groups (MSN-SH). These were chosen specifically due to their high affinity to copper and silver ions, which were used as antimicrobial payloads and could be incorporated into the mesoporous structure through favorable host−guest interactions, allowing us to find the most favorable combinations to achieve antimicrobial efficacy against various microbes on dry or semidry high-touch surfaces. The antimicrobial MSNs were firmly immobilized on stainless steel through a simple two-step spray-coating process. First, the stainless steel surfaces are primed with sprayable polyelectrolyte solutions acting as adhesion layers, and then, the loaded nanoparticle dispersions are spray-coated on top. The employed polyelectrolytes were selected and functionalized specifically to adhere well to stainless steel substrates while at the same time being complementary to the MSN surface groups to enhance the adhesion, wettability, homogeneity, and stability of the coatings. The antimicrobial properties of the nanoparticle suspension and the coatings were tested against three commonly found pathogenic bacteria, Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli, as well as a fungal pathogen, Candida albicans. Especially MSN-SH loaded with silver ions showed excellent antimicrobial efficacy against all tested pathogens under application-relevant, (semi)dry conditions. The findings obtained here facilitate our understanding of the correlation between the surface properties, payloads, and antimicrobial activity and show a new pathway toward simple and easily deployable solutions to combat the spread of pathogens with the help of sprayable antimicrobial surface coatings.
KW - Mesoporous silica nanoparticles
KW - Thin films
KW - Antimicrobial coatings
KW - Spray-coating
KW - Infectious diseases
KW - Pathogen transmission
KW - High-touch surfaces
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626269
DO - https://doi.org/10.1021/acsami.4c18916
SN - 1944-8252
SP - 1
EP - 13
PB - ACS Publications
CY - Washington, DC
AN - OPUS4-62626
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ruehle, Bastian
T1 - Natural language processing for automated workflow and knowledge graph generation in self-driving labs
N2 - Natural language processing with the help of large language models such as ChatGPT has become ubiquitous in many software applications and allows users to interact even with complex hardware or software in an intuitive way. The recent concepts of Self-Driving Labs and Material Acceleration Platforms stand to benefit greatly from making them more accessible to a broader scientific community through enhanced user-friendliness or even completely automated ways of generating experimental workflows that can be run on the complex hardware of the platform from user input or previously published procedures. Here, two new datasets with over 1.5 million experimental procedures and their (semi)automatic annotations as action graphs, i.e., structured output, were created and used for training two different transformer-based large language models. These models strike a balance between performance, generality, and fitness for purpose and can be hosted and run on standard consumer-grade hardware. Furthermore, the generation of node graphs from these action graphs as a user-friendly and intuitive way of visualizing and modifying synthesis workflows that can be run on the hardware of a Self-Driving Lab or Material Acceleration Platform is explored. Lastly, it is discussed how knowledge graphs – following an ontology imposed by the underlying node setup and software architecture – can be generated from the node graphs. All resources, including the datasets, the fully trained large language models, the node editor, and scripts for querying and visualizing the knowledge graphs are made publicly available.
KW - Natural Language Processing
KW - Large Language Models
KW - Self-Driving Labs
KW - Materials Acceleration Platforms
KW - Workflows
KW - Nanomaterials
KW - Advanced Materials
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631947
UR - https://github.com/BAMresearch/MAPz_at_BAM/tree/main/Minerva-Workflow-Generator
DO - https://doi.org/10.1039/d5dd00063g
SN - 2635-098X
SP - 1
EP - 10
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-63194
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kamdem Tamo, Arnaud
A1 - Doench, Ingo
A1 - Deffo, Gullit
A1 - Jiokeng, Sherman Lesly Zambou
A1 - Doungmo, Giscard
A1 - Fotsop, Cyrille Ghislain
A1 - Temgoua, Ranil Clement Tonleu
A1 - Montembault, Alexandra
A1 - Serghe, Anatoli
A1 - Njanja, Evangeline
A1 - Tonle, Ignas Kenfack
A1 - Osorio-Madrazo, Anayancy
T1 - Lignocellulosic biomass and its main structural polymers as sustainable materials for (bio)sensing applications
N2 - (Bio)sensors are integral to various aspects of daily life, contributing to safety, monitoring, and awareness. In modern sensor devices, polymers play an important role, with increasing interest in bio-based materials. Biopolymers, unlike their synthetic counterparts, are abundant in nature and exhibit interesting functional properties that make them highly suitable as biomaterials for sensor technologies. Enhancing sensor performance to achieve a rapid response to stimuli is a key objective in sensor development. Lignocellulosic biomass (LCB) from plants holds promise in meeting such requirements due to its high surface area, tunable surface characteristics (including diverse pore sizes and morphologies), flexibility, printability, low density, and favorable physicochemical and thermal properties. Growing research in recent decades has focused on lignocellulosic composite materials due to their functional and environmentally friendly attributes. This review focuses on the valorization of lignocellulosic biomass and its three main biopolymer constituents (cellulose, hemicellulose, and lignin) for the development of electrochemical (bio)sensors. It also explores the macromolecular structure, sources, and inherent properties of LCB, with emphasis on the three main biopolymers and their applications in sensor technologies. Recent advances in the use of LCB and its structural biopolymers as materials for (bio)sensing applications are described and reviewed. The challenges associated with using these biomaterials in electroanalytical applications are also discussed, along with the exploration of their future potential for developing high-performance sensing technologies.
KW - Chemical safety
KW - Material safety
KW - Quality ensurance
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637230
DO - https://doi.org/10.1039/d5ta02900g
SN - 2050-7496
SP - 1
EP - 69
PB - The Royal Society of Chemistry
AN - OPUS4-63723
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Bruno, Francesco
A1 - Fiorucci, Letizia
A1 - Vignoli, Alessia
A1 - Meyer, Klas
A1 - Maiwald, Michael
A1 - Ravera, Enrico
T1 - pyIHM: Indirect Hard Modeling, in Python
N2 - NMR is a powerful analytical technique that combines an exquisite qualitative power, related to the unicity of the spectra of each molecule in a mixture, with an intrinsic quantitativeness, related to the fact that the integral of each peak only depends on the number of nuclei (i.e., the amount of substance times the number of equivalent nuclei in the signal), regardless of the molecule. Signal integration is the most common approach in quantitative NMR but has several drawbacks (vide infra). An alternative is to use hard modeling of the peaks. In this paper, we present pyIHM, a Python package for the quantification of the components of NMR spectra through indirect hard modeling, and we discuss some numerical details of the implementation that make this approach robust and reliable.
KW - Algorithms
KW - Chemical Structure
KW - Deconvolution
KW - Mixtures
KW - NMR spectroscopy
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626793
DO - https://doi.org/10.1021/acs.analchem.4c06484
SN - 1520-6882
VL - 97
IS - 8
SP - 4598
EP - 4605
PB - ACS Publications
CY - Washington D.C.
AN - OPUS4-62679
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dorgerloh, Ute
A1 - Becker, Roland
A1 - Freeling, Finnian
A1 - Scheurer, Marco
A1 - Gökçe, Emine
A1 - Strack, Katrin
A1 - Sommerfeld, Thomas
A1 - Sauer, Andreas
A1 - Schneider, Jonas
A1 - Härtel, Christoph
A1 - Valkov, Vassil
A1 - Moser, Lukas
A1 - Geiß, Sabine
A1 - Junginger, Sabine
A1 - Schlittenbauer, Linda
A1 - Suess, Elke
A1 - Ruth, Katinka
T1 - Standardising the quantification of trifluoroacetic acid in water: Interlaboratory validation trial using liquid chromatography-mass spectrometric detection (LC–MS/MS)
N2 - The concentration of trifluoroacetic acid in surface and groundwaters and drinking water is subject of increasing concern. Since there is no standardised procedure available, German standardisation body DIN has initiated the first draft standard using liquid chromatography with tandem mass spectrometry (LC–MS/MS) after direct injection for the concentration range between ≥ 0.1 and 3 µg/L. Herein, the interlaboratory comparison as final validation step involving 12 expert laboratories from Germany and Switzerland is described. Two groundwaters, two surface waters, a drinking water, a rainwater, and two fortified groundwater samples displayed relative repeatability standard deviations between 3 and 7% and relative reproducibility standard deviation between 6 and 20% and were included in the draft standard DIN 38407-53.
KW - TFA Trifluoroacetic acid
KW - LC/MS-MS
KW - Validation trial
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632376
DO - https://doi.org/10.1007/s00769-025-01640-2
SN - 0949-1775
SP - 1
EP - 4
PB - Springer
CY - Berlin
AN - OPUS4-63237
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Michalska, Karina
A1 - Heiermann, Monika
A1 - Lühr, Carsten
A1 - Meermann, Björn
A1 - Pecenka, Ralf
A1 - Schulz, Andreas
A1 - Langhammer, Nicole
A1 - Theuerl, Susanne
A1 - Prochnow, Annette
T1 - Potentials of typical plant species from rewetted fenlands for the supply of strategic elements
N2 - Rewetting of peatlands requires the development of new biomass utilization pathways. The supply of strategic elements with key importance for the development of priority technologies, such as germanium (Ge), silicon (Si) and rare earth elements, from fenland plants is one option. To provide a first estimation of the potential, concentrations of strategic elements were determined in nine biomass samples covering typical fenland vegetation in northeast Germany. Subsequently, a simplified estimation of potential revenue from strategic element recovery was made. The analysed plant species can be classified as high or intermediate Si plant accumulators with highest contents of more than 16.0 g Si kg−1 dry mass (DM) in sedges and common reeds. Ge concentrations were lower with reed canary grass containing the highest amounts of 465.3 µg Ge kg−1 DM. Simultaneous acquisition of Ge and Si could provide higher total element yields and revenues of up to 500 $ ha−1. In contrast, the potentials for supplying rare earth elements appeared to be very low, with common reed containing the highest sum of rare earth elements of 437.4 µg kg−1 DM. Biomass from rewetted fenlands is capable of accumulating strategic elements. More knowledge is required to understand the factors affecting their accumulation.
KW - Recycling
KW - Fenlands
KW - Strategic elements
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635631
DO - https://doi.org/10.1038/s41598-025-05180-0
SN - 2045-2322
VL - 15
IS - 1
SP - 1
EP - 14
PB - Springer Science and Business Media LLC
AN - OPUS4-63563
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Bourgon, Nicolas
A1 - Oelze, Marcus
A1 - Roberts, Patrick
T1 - Less is more: Limiting semi-invasive sampling for multi-isotope analyses and increasing data output from single aliquot samples
N2 - Developments in multi-isotope applications now enable the production of direct and precise life history data of studied archeological and paleoanthropological specimens, with analysis of tooth enamel proving particularly powerful in deep-time preservation contexts. However, the increasing amount of sample material necessary too-often compromises the specimen's structural integrity. Finding ways of minimizing semi-invasive sampling while maximizing produced data thus becomes increasingly crucial. In this study, we examine ways of optimizing sample use for state-of-the-art isotope measurements of enamel-bound zinc (δ66Zn), an increasingly used method in multi-isotope archeological research. We show that certain desolvating nebulizer introduction systems can be used to measure δ66Zn with high efficiency and accuracy using less than half the usual sample size. Moreover, we demonstrate that remaining samples subjected to typical pretreatments used for tooth enamel carbonate (δ13C and δ18O) studies can be safely used without alterations to δ66Zn values. Similarly, we highlight that the often-discarded matrix fraction from zinc chromatography can be utilized for further analyses, such as measurements of 87Sr/86Sr ratios. Our results underscore the possibility of extracting the maximum information from specimens while altogether avoiding or significantly reducing semi-invasive sampling.
KW - Multi-isotope
KW - Zinc isotope analysis
KW - Tooth enamel
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637986
DO - https://doi.org/10.1016/j.jas.2025.106308
SN - 0305-4403
VL - 180
SP - 1
EP - 8
PB - Elsevier Ltd.
AN - OPUS4-63798
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scharek, Vera M.
A1 - Pfeifer, Jens
A1 - Vogl, Jochen
A1 - Traub, Heike
A1 - Meermann, Björn
T1 - Tin fractionation analysis in sediment samples via on-line ID ETV/ICP-MS
N2 - We report a quantification approach for directly determining total tin and tin-based pollutants/species in sediments via electrothermal vaporization/inductively coupled plasma-mass spectrometry (ETV/ICP-MS) utilizing an on-line isotope dilution mass spectrometry (IDMS) approach. The method was developed and validated using an estuarine sediment reference material (BCR-277R), yielding a recovery of 106%. A relative standard deviation (RSD) of 14%, comparable to published data using a similar method, was obtained. A limit of quantification (LOQ) was estimated at 0.008 mg Sn kg−1 and sufficient for quantifying the total tin mass fraction of surface sediments along the tidal River Elbe course. Hereby, a decrease towards the river mouth, presumably due to dilution effects by less polluted marine sediment, was observed. Besides total tin, monitoring of organotin compounds (OTCs)/species is of interest in sediments due to their toxic effects on aquatic life. The method’s capability was extended by separating an OTC fraction in a sediment certified reference material (CRM) through the ETV temperature program. While spiking experiments with OTC standards confirmed the assignment, only a small fraction of the total certified OTC amount (3%), likely due to matrix effects, was recovered. However, applying the method to real-world samples, OTCs were detectable along the River Elbe course. By this, we demonstrated the potential of our method as a complementary fast-screening approach to species-specific analysis procedures.
KW - ETV
KW - Sn-Speciation
KW - Sediment
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640137
DO - https://doi.org/10.1007/s00216-025-06064-y
SN - 1618-2642
SP - 1
EP - 10
PB - Springer Science and Business Media LLC
AN - OPUS4-64013
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Feord, Helen K.
A1 - Trautwein-Schult, Anke
A1 - Keuschnig, Christoph
A1 - Ostrzinski, Anne
A1 - Peter, Elisa K.
A1 - Jaeger, Carsten
A1 - Lisec, Jan
A1 - Mourot, Rey
A1 - Peters, Ravi Sven
A1 - Çiftçi, Ozan
A1 - Tranter, Martyn
A1 - Anesio, Alexandre M.
A1 - Becher, Dörte
A1 - Benning, Liane G.
T1 - Algae-dominated metaproteomes uncover cellular adaptations to life on the Greenland Ice Sheet
N2 - Eukaryotic algae-dominated microbiomes thrive on the Greenland Ice Sheet (GrIS) in harsh environmental conditions, including low temperatures, high light, and low nutrient availability. Chlorophyte algae bloom on snow, while streptophyte algae dominate bare ice surfaces. Empirical data about the cellular mechanisms responsible for their survival in these extreme conditions are scarce. This knowledge gap was addressed by quantifying proteins for both algal taxa from samples on the southern margin of the GrIS. We show that the streptophyte glacier ice algae have a relative enrichment in proteins involved in environmental signaling and nutrient transport, indicative of cellular readiness to dynamically respond to extreme GriS environmental cues, linked, for example, to photoprotection and the rapid update of scarce nutrients. In contrast, the chlorophyte snow algae have a high abundance of proteins linked to lipid and nitrogen metabolisms, providing evidence for the biological processes sustaining the cellular carbon and nitrogen stores necessary for survival in an oligotrophic environment. We also identify proteins in both taxa linked to the synthesis and breakdown of key cellular pigments. Our study gives novel insights into the cellular biology of these algae and their adaptation to extreme environments.
KW - Metabolic profiling
KW - Mass spectrometry
KW - Ice algae
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641037
DO - https://doi.org/10.1038/s41522-025-00770-2
SN - 2055-5008
VL - 11
IS - 1
SP - 1
EP - 11
PB - Springer Science and Business Media LLC
AN - OPUS4-64103
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schannor, Mathias
A1 - Oelze, Marcus
A1 - Traub, Heike
A1 - He, Yubei
A1 - Schmidt, Robin
A1 - Heidemann, Luisa
A1 - Savic, Lynn Jeanette
A1 - Vogl, Jochen
A1 - Meermann, Björn
T1 - Advancing Biomarker Research: In Situ Cu Isotope Analysis in Liver Tumors by LA-MC-ICP-MS
N2 - Stable metal isotopes have received increasing attention as medical biomarkers due to their potential to detect changes in metal metabolism related to diseases. In particular, copper stable isotopes are a powerful tool to identify isotopic variation between tumors and healthy tissue, suggesting application in cancer diagnosis. However, potential mechanisms causing isotope fractionation, such as redox- or bond-forming reactions and interactions of metals during transmembrane import and export, are less well understood. Here, we established an in situ method using laser ablation-multicollector-inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) to advance our understanding of the underlying processes responsible for isotope fractionation between normal and diseased tissues. Gelatin-based bracketing standards and quality control reference materials, crucial for laser ablation analysis, were developed to allow correction for instrumentally induced isotope fractionation during LA-MC-ICP-MS analysis. Using such matrix-matched standards, the method achieved intermediate precisions for delta values of better than 0.15 ‰ (2 s) for inorganic reference materials and of better than 0.17 ‰ (2 s) for biological reference materials. The developed routine was tested on rabbit VX2 liver tumor samples, a model system resembling human hepatocellular carcinoma (HCC) used to study liver cancer. In situ Cu isotope compositions between healthy (𝛿65/63NIST976(Cu) = −1.5 ‰ to 0.2 ‰) and tumorous (𝛿65/63NIST976(Cu) = 0.0 ‰ to 1.3 ‰) liver tissue show distinct differences in their isotope ratios. The observed isotopic dichotomy is consistent with previous solution-based MC-ICP-MS work, showing enrichment of heavy 65Cu in cancer biopsies relative to healthy tissue.
KW - Biomarker
KW - Laser Ablation
KW - Reference Material
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626865
DO - https://doi.org/10.1021/acs.analchem.4c05626
SN - 1520-6882
VL - 97
IS - 8
SP - 4425
EP - 4432
PB - American Chemical Society (ACS)
AN - OPUS4-62686
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Löwa, N.
A1 - Golusda, L.
A1 - Paclik, D.
A1 - Traub, Heike
A1 - Schannor, Mathias
A1 - Saatz, Jessica
A1 - Freise, C.
A1 - Taupitz, M.
A1 - Siegmund, B.
A1 - Kühl, A. A.
A1 - Wiekhorst, F.
T1 - Magnetic particle spectroscopy for Eu-VSOP quantification in intestinal inflammation: Distinguishing nanoparticle signals from dietary contamination
N2 - Magnetic nanoparticles are gaining increasing attention as a promising alternative to gadolinium-based contrast agents in magnetic resonance imaging, primarily due to their low toxicity. In this study, we investigated the use of magnetic iron oxide nanoparticles in mouse models of intestinal inflammation to assess their potential for detecting changes in the extracellular matrix. For magnetic quantification, we employed magnetic particle spectroscopy, which offers high sensitivity and minimal interference from biological tissue. However, we observed significant variations in magnetic signals within the intestine, as well as measurable signals in control animals, indicating possible magnetic contamination. By doping the nanoparticles with europium, we were able to confirm this suspicion through quantitative elemental analysis. Examination of mouse feed and feces allowed us to identify the source of contamination. Based on these findings, we developed a method to reliably distinguish genuine signals of magnetic nanoparticles from those caused by external magnetic contaminations. This approach is essential to ensure reliable results in future diagnostic and preclinical research.
KW - ICP-MS
KW - Nanoparticle
KW - Magnetic particle spectroscopy
KW - Quantification
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642238
DO - https://doi.org/10.1039/D5NA00452G
SN - 2516-0230
IS - 00452
SP - 1
EP - 10
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64223
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lozano-Martín, Daniel
A1 - Kipphardt, Heinrich
A1 - Khanipour, Peyman
A1 - Tuma, Dirk
A1 - Horrillo, Alfonso
A1 - Chamorro, César R.
T1 - Impact of hydrogen addition, up to 20 % (mol/mol), on the thermodynamic (p, ρ, T) properties of a reference high-calorific natural gas mixture with significant ethane and propane content
N2 - Injecting hydrogen into the natural gas grid supports gradual decarbonization. To check the accuracy of equations of state for hydrogen-enriched natural gas mixtures, precise density data from well-characterized reference mixtures are essential. In a prior study, we provided experimental measurements for a natural gas constituted mainly of methane and for two derived hydrogen-enriched mixtures. In the present study, being the second and final part of our investigation, density measurements for a high-calorific natural gas with significant ethane and propane content, along with two hydrogen-enriched variants (10 and 20 mol-% hydrogen) are provided. The mixtures are gravimetrically prepared following ISO 6142-1. Density measurements, conducted with a single-sinker densimeter at temperatures from (260–350) K and pressures up to 20 MPa, are compared with three equations of state: AGA8-DC92, GERG-2008, and an improved GERG-2008. Results indicate that all models perform better for methane-dominant mixtures than for those containing heavier hydrocarbons.
KW - Hydrogen-enriched natural gas
KW - High-pressure density
KW - Reference equation of state
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633371
DO - https://doi.org/10.1016/j.ijhydene.2025.05.173
SN - 0360-3199
VL - 140
SP - 256
EP - 271
PB - Elsevier BV
CY - Amsterdam
AN - OPUS4-63337
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zhuang, Yiling
A1 - Haderlein, Stefan B.
A1 - Hagemann, Nikolas
A1 - Grafmüller, Jannis
A1 - Gogler, Karolin
A1 - Paul, Andrea
A1 - Fink, Friedrich
A1 - Spahr, Stephanie
T1 - Activation of persulfate by biochar and iron: role of biochar pyrolysis conditions and ash amendments
N2 - Redox-active biochars can enhance contaminant transformation in persulfate-based Fenton-like water treatment by facilitating Fe(III) reduction to Fe(II). However, biochar properties vary greatly depending on both feedstock selection and pyrolysis conditions. Best suited biochars for Fe(III) reduction and persulfate activation have yet to be identified. Here, we investigated eight biochars for their ability to activate persulfate with Fe(III) to transform N,N-diethyl-m-toluamide (DEET) in water. Four of the biochars were produced from beech wood under different pyrolysis conditions (450–750 °C, high and low nitrogen flow rate in the reactor) and four biochars were produced from softwood amended with 0 – 43 weight percent (wt%) wood ash prior to pyrolysis at 500 °C. Beech wood biochar produced at 450 °C transformed DEET most efficiently with a half-life time of 39 ± 4 min, likely due to the high concentration of surface oxygen functional groups and persistent free radicals that accelerated Fe(III) reduction and formation of reactive species. Among the ash-amended biochars, biochar with 16 wt% ash amendment showed the most efficient DEET transformation with a half-life time of 27 ± 0.6 min, which is 10-times faster compared to a non-ash-amended biochar produced from the same biomass under similar pyrolysis conditions. Ash amendment led to the formation of crystalline iron minerals in biochars, which likely promoted Fe(III) reduction and persulfate activation. Our results highlight the potential for fine-tuning the redox properties of biochar, e.g., by ash amendment to a woody feedstock, enabling tailored performance for specific water treatment applications.
KW - Persistent free radicals
KW - Redox-active moieties
KW - Fenton-like systems
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634504
DO - https://doi.org/10.1016/j.seppur.2025.133634
SN - 1383-5866
VL - 374
SP - 1
EP - 8
PB - Elsevier B.V.
AN - OPUS4-63450
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sowoidnich, Kay
A1 - Pätzold, Stefan
A1 - Ostermann, Markus
A1 - Sumpf, Bernd
A1 - Maiwald, Martin
T1 - Qualitative and quantitative soil characterization on an agricultural field using a portable shifted excitation Raman difference spectroscopy instrument
N2 - Site-specific farmland management requires comprehensive information about the soil status to derive informed treatment decisions, e.g. for liming or fertilizer recommendations. Standard laboratory methods relying on sample collection have only limited ability to adequately capture the spatial variability of typical agricultural fields. Here, on-site analytical techniques with the potential to measure the soil properties on a substance-specific level and at the required spatial resolution could be very beneficial. Raman spectroscopy is a very promising technique for this purpose as it provides a molecular fingerprint of soil constituents. However, intrinsic soil fluorescence and daylight interference can be major issues masking characteristic Raman signals. Here, we apply an in-house developed portable shifted excitation Raman difference spectroscopy (SERDS) instrument based on a dual-wavelength diode laser emitting around 785 nm to effectively separate the Raman signals of soil from such interferences. SERDS investigations on a selected agricultural field in Germany demonstrate that the Raman spectroscopic signature of 9 soil minerals and organic carbon could successfully be separated from intense backgrounds. Using partial least squares regression against reference analyses, a successful prediction of the soil carbonate (R2 = 0.86, root mean squared error of cross validation RMSECV = 2.49%) and soil organic carbon content (R2 = 0.89, RMSECV = 0.32%) as important soil parameters is realized. The results obtained on-site with the portable instrument were confirmed by SERDS laboratory experiments of collected soil samples thus highlighting the capability and reliability of portable SERDS as promising and complementary tool for precision agriculture
KW - XRF
KW - Raman spectroscopy
KW - Soil
KW - SERDS
KW - Precision agriculture
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634597
DO - https://doi.org/10.1039/d5an00178a
SN - 0003-2654
VL - 150
IS - 13
SP - 2934
EP - 2944
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-63459
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Golub, Tino Petar
A1 - Meyer, Klas
A1 - Paul, Andrea
A1 - Kipphardt, Heinrich
A1 - Tuma, Dirk
T1 - Exploring the potential of a setup for combined quantification of hydrogen in natural gas – Raman and NMR spectroscopy
N2 - An accurate measurement of the amount fraction of hydrogen in gas mixtures is mandatory for practical applications, requiring methods that are fast, continuous, robust, and cost-effective. This study compares the performance of Raman and benchtop NMR process spectroscopy for determining the hydrogen amount fraction in gas mixtures. A setup was designed to integrate both techniques, enabling measurements of the same sample.
Tests were conducted with gravimetrically prepared gas mixtures of reference quality ranging from 1.20 cmol/mol to 85.83 cmol/mol of hydrogen. The results demonstrate that Raman spectroscopy provides superior performance, with a minimal root mean square error (RMSE) of 0.22 cmol/mol and excellent linearity. In contrast, benchtop NMR spectroscopy faced challenges, such as overlapping peaks and longer measurement times, resulting in a higher RMSE of 0.71 cmol/mol. Raman spectroscopy proves to be particularly well-suited for
practical applications due to its high accuracy and linearity. Meanwhile, benchtop NMR spectroscopy holds potential for future enhancements through ongoing technological advances, such as higher magnetic field strengths. In summary, the results from our study indicate that Raman spectroscopy is already a serviceable method for precise hydrogen quantification, whereas benchtop NMR spectroscopy can be attributed potential for future applications.
KW - Hydrogen amount fraction
KW - Raman spectroscopy
KW - NMR spectroscopy
KW - Field applicability
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610093
DO - https://doi.org/10.1016/j.saa.2024.125087
SN - 1386-1425
VL - 325
SP - 1
EP - 9
PB - Elsevier B.V.
CY - Amsterdam
AN - OPUS4-61009
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Thiele, Isabel
A1 - Weiske, Björn
A1 - Riedel, Sebastian L.
A1 - Meyer, Klas
T1 - On-line monitoring of polyhydroxyalkanoate extraction by low-field nuclear magnetic resonance spectroscopy
N2 - The use of low-field nuclear magnetic resonance (NMR) spectroscopy enables real-time reaction monitoring in contrast to time-consuming gas chromatography or off-line high-field NMR measurements. In this study, NMR spectroscopy is demonstrated as a novel process analytical technology (PAT) tool in the downstream processing of polyhydroxyalkanoate (PHA) biopolymers. On-line NMR spectroscopy measurements were performed using a Spinsolve 43 Carbon Ultra instrument in a fully automated mode with a flow-assembly based on PTFE tubing. Single-scan NMR spectra were acquired for real-time monitoring of the extraction process of the PHA copolymer poly(hydroxybutyrate-co-hydroxyhexanoate) with 13.5 mol.% hydroxyhexanoate [P(HB-co-13.5 mol.%HHx)] from Ralstonia eutropha biomass using chloroform or acetone as PHA solvents at lyophilized cell loadings of 20–120 g L 1. The reproducibility and reliability of low-field NMR spectroscopy was comparable to high-field NMR spectroscopy, with superior performance in terms of time. The correlation between the results of on-line monitoring using low-field NMR spectroscopy and off-line analysis using gas chromatography (GC) showed a correlation coefficient of >94 %. The versatility of low-field NMR spectroscopy for elucidating reaction kinetics, facilitating endpoint determination and accelerating extraction processes by maximizing solubility is highlighted as plateau values were reached within 6–10 min for chloroform and acetone, respectively. This novel low-field NMR spectroscopy application promotes a new monitoring approach for downstream PHA processing and supports process development and optimization.
KW - Polyhydroxyalkanoate
KW - Extraction
KW - NMR
KW - Ralstonia eutropha
KW - Downstream processing
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624215
DO - https://doi.org/10.1016/j.polymdegradstab.2025.111188
SN - 1873-2321
VL - 233
SP - 1
EP - 10
PB - Elsevier Ltd.
CY - Amsterdam
AN - OPUS4-62421
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mervič, Kristina
A1 - Azimzada, Agil
A1 - Bayat, Mehmet Emin
A1 - Šala, Martin
A1 - Meermann, Björn
T1 - CO2-based matrix-independent carbon quantification approach for single microplastic-ICP-MS analysis
N2 - This study presents a new CO2-based, matrix-independent calibration approach for size determination of microplastic (MP) particles using single particle inductively coupled plasma-mass spectrometry (sp-ICP-MS). By incorporating a CO2 gas calibration approach and upon adjusting the flow rates, an accurate size determination of MPs between 2 and 7 μm was enabled. Scanning electron microscopy (SEM) was successfully applied for method validation. The CO2 gas calibration curves exhibited excellent linearity and reproducibility, with minimal matrix effects across different sample types and matrices, including river water and saline solutions. This CO2-based approach eliminates the limitations of matrix- and size-dependent calibrations, enabling robust and accurate size determinations of MPs. This advancement represents a significant step forward in the analytical capabilities for MPs, paving the way for improved environmental monitoring and assessment of plastic pollution.
KW - sp-ICP-MS
KW - Microplastic
KW - New calibration strategy
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633049
DO - https://doi.org/10.1007/s00216-025-05934-9
SN - 1618-2642
SP - 1
EP - 11
PB - Springer
CY - Berlin
AN - OPUS4-63304
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tobias, Charlie
A1 - Gehrenkemper, Lennart
A1 - Bernstein, Thomas
A1 - Schlau, Sven
A1 - Simon, Fabian
A1 - Röllig, Mathias
A1 - Meermann, Björn
A1 - von der Au, Marcus
T1 - Development of a fully automated slurry sampling introduction system for GF-AAS and its application for the determination of cadmium in different matrices
N2 - element analysis, offering high sensitivity and precision. However, its effectiveness is limited by sample preparation challenges for solid samples like soils and microplastics. Traditional methods include sample preparation, such as digestion, which is time-consuming and involves reagents, like acids, contributing to measurement uncertainty and higher carbon footprints. Slurry sampling allows direct analysis of suspensions, offering a more efficient alternative. However, maintaining suspension stability is challenging, requiring robust autosampler systems to streamline the process and enhance analytical performance.
Results: We present a novel autosampler extension for slurry sample introduction into GF-AAS. This system ensures suspension stability with a stirring device and closed vessels to prevent evaporation and contamination, incorporating a cooling unit to reduce solvent and analyte losses. It installs and removes in minutes without
additional connections. Validation with cadmium analysis in BAM-U110 (Soil) and BAM-H010 (ABS) showed high reliability. For BAM-U110 (Soil), we achieved recovery rates of 94 % ± 13 % in water suspension. The recovery rate for BAM-H010 (ABS) was 104 % ±11 % in acetonitrile suspension. These results demonstrate the system’s robustness, versatility, and accuracy for different matrices.
Significance:
The autosampler extension helps solve key problems in trace element analysis of solid samples, making the process faster and more accurate. It works well with complex materials, making it useful for areas like microplastic or nanoparticle analysis. This improvement also helps meet regulations for monitoring environ mental and polymer samples, offering a reliable and flexible tool for high-throughput analysis with fewer errors.
KW - Slurry AAS
KW - Soil
KW - Cd
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618531
DO - https://doi.org/10.1016/j.aca.2024.343460
SN - 0003-2670
VL - 1335
SP - 1
EP - 7
PB - Elsevier BV
AN - OPUS4-61853
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Vermeeren, Sarah
A1 - Witzler, Markus
A1 - Makarow, Ramona
A1 - Engelhard, Carsten
A1 - Kaul, Peter
T1 - Multivariate evaluation method for the detection of pest infestations on plants via VOC analysis using gas chromatography mass spectrometry
N2 - Volatile organic compounds (VOCs) play an important role in the defense against pest infestations on plants. The analysis of these VOCs using gas chromatography mass spectrometry (GC-MS) enables the detection of pests by analyzing the VOC composition (VOC profiles) for specific patterns and markers. The analysis of such complex datasets with high biovariability poses a particular challenge. For this reason, a multivariate evaluation method based on a self-written Python script, using principal component analysis (PCA) and linear discriminant analysis (LDA), was developed and tested for functionality using a dataset, which has been evaluated manually and has identified five specific markers (2,4-dimethyl-1-heptene, 3-carene, alpha-longipinene, cyclosativene, and copaene) for Anoplophora glabripennis (ALB) infestation on Acer trees. The results obtained in the present study did not only match the manually evaluated results, but lead to further insight into the dataset. Another sesquiterpene which is assumed to be alpha-zingiberene was identified as an ALB specific marker in addition to 2,4-dimethyl-1-heptene and 3-carene. Furthermore, the European native beetle species goat moth Cossus cossus (CC) and poplar long-horned beetle Saperda carcharias (SC) were also analyzed for their VOCs to differentiate ALB specific VOC from other pest infestations. This comparison lead to the conclusion that the compounds alpha-longipinene, cyclosativene, and copaene are not specific for ALB but for pest infestation in general. It was possible to identify not only specifically produced VOCs, but also differences in concentrations that arise specifically during ALB infestation. Therefore, the evaluation method for the detection of plant pests presented in this study represents a time-saving alternative to conventional non computing methods, which in addition provides more detailed results.
KW - Mass Spectrometry
KW - Gas Chromatography
KW - Volatile organic compounds
KW - Pest infestation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639526
DO - https://doi.org/10.1038/s41598-025-11607-5
SN - 2045-2322
VL - 15
IS - 1
SP - 1
EP - 10
PB - Springer Science and Business Media LLC
AN - OPUS4-63952
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Braun, Jennifer
A1 - Engelhard, Carsten
A1 - Kaul, Peter
T1 - Optimized fast gas chromatography coupled with proton-transfer-reaction time-of-flight mass spectrometry for the selective near real-time analysis of herbivore-induced plant volatiles
N2 - The analysis of herbivore-induced plant volatiles (HIPVs) is essential for understanding plant-environment interactions and defense strategies against herbivores. Proton transfer reaction time-of-flight mass spectrometry (PTR–TOF–MS) is a powerful analytical tool that enables real-time monitoring and quantification of diverse groups of HIPVs. However, the PTR–TOF–MS technique is constrained in its ability to effectively differentiate between isomers. When analyzing complex mixtures of HIPVs, the separation of isomers becomes crucial as major compound classes such as terpenes comprise thousands of isomers. In this study, we present an optimized fast gas chromatography (fastGC) based on a modified version of the commercially available fastGC add-on integrated into a mobile PTR–TOF. The system was optimized for the analysis of emissions from enclosed trunks of Acer platanoides infested by Anoplophora glabripennis (Motschulsky), commonly known as Asian longhorned beetle (ALB). The development of fastGC was primarily focused on the sesquiterpenes α-longipinene, cyclosativene and α-copaene, which serve as strong indicators of ALB infestation. These sesquiterpenes were separated in less than three minutes, with intra-day retention time RSD < 0.6 % and resolutions of 2.6 ± 0.3 and 1.3 ± 0.2. In comparison to the original system, the optimized fastGC demonstrates more than tripled sesquiterpene resolution, twice the sensitivity relative to direct inlet mode, and an approximately 10 % reduction in total analysis time. The optimized fastGC–PTR–TOF allows for near real-time analysis of complex mixtures of biogenic VOCs, making it a powerful tool for environmental monitoring, integrated pest management, and forest protection.
KW - Mass Spectrometry
KW - PTR-TOF-MS
KW - Gas Chromatography
KW - Herbivore-induced plant volatiles
KW - Sesquiterpenes
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639513
DO - https://doi.org/10.1016/j.chroma.2025.466236
SN - 0021-9673
VL - 1759
SP - 1
EP - 16
PB - Elsevier B.V.
AN - OPUS4-63951
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Azimzada, Agil
A1 - Meermann, Björn
T1 - AF4/ICP-ToF-MS for the investigation of species-specific adsorption of organometallic contaminants on natural colloidal particles
N2 - Organotin (OT) compounds, while crucial in many industrial applications, pose substantial risks to the environment and human health. The toxicity and environmental behaviour of OTs depend on their chemical form, i.e., the type and number of organic substituents. Each species thus exhibits distinct toxicity profiles and varying binding affinities to environmental colloids, which influence their mobility, bioavailability, and environmental impacts. To date, however, most studies addressed speciation and colloidal characterization separately, leaving the combined determinations of organometallics along with their carrier colloids largely elusive. Here, we develop and validate an on-line measurement system to quantify the adsorption dynamics of 10 OT species on natural colloidal particles (<500 nm). The approach integrates a versatile fractionation technique (AF4), with a state-of-the-art multi-element analyzer (ICP-ToF-MS), achieving Sn detection limits as low as 6.0 ng/L. The method separates colloid-free OT species from those bound to colloids and enables the determination of OT interactions with distinct colloidal fractions. Validated in both fractionation and detection, the method provides reliable data that could elucidate the species-specific and temporal aspects of species-colloids adsorption processes. The results feature comparative studies of 10 OT species, offering critical insights into OT mobility and distribution in environmental systems.
KW - Fractionation
KW - Speciation
KW - Adsorption
KW - Colloids
KW - Organotin
KW - AF4
KW - Nanoparticle characterization
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625244
DO - https://doi.org/10.1016/j.jhazmat.2025.137320
SN - 1873-3336
VL - 488
SP - 1
EP - 11
PB - Elsevier B.V.
AN - OPUS4-62524
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlögl, Johanna
A1 - Krappe, Alexander R.
A1 - Fürstenwerth, Paul C.
A1 - Brosius, Amelie L.
A1 - Fasting, Carlo
A1 - Hoffmann, Kurt F.
A1 - Resch-Genger, Ute
A1 - Eigler, Siegfried
A1 - Steinhauer, Simon
A1 - Riedel, Sebastian
T1 - Luminescent Perhalofluoro Trityl Radicals
N2 - In this proof-of-concept study, we show that polyfluorinated trityl radicals with the, to this date, highest fluorination grade can be accessed in quantitative yields in a straightforward manner starting from the perfluorinated trityl cation. The trityl skeleton is functionalized with trimethylsilyl halides to yield perhalofluoro trityl cations, which are subsequently reduced using commercial zinc powder. In this way, we prepare three perhalofluoro trityl radicals and analyze the impact of the fluorine ligands on their electro-optical properties, revealing some interesting trends. In comparison to literature-known polychlorinated trityl radicals, the new polyfluorinated derivatives exhibit substantially higher fluorescence quantum yields, longer luminescence lifetimes, and an expanded emission range that extends into the yellow spectral region. They further display enhanced photostability under light irradiation. In radical-stained polystyrene nanoparticles, an additional broad emission band in the red−NIR wavelength region is observed, which is attributed to excimer formation. Finally, the stability of the new radicals is investigated under ambient conditions, showing the slow conversion with atmospheric oxygen yielding the respective peroxides, which are characterized by single-crystal X-ray diffraction. All in all, our study extends the present scope of luminescent trityl radicals, as the functionalization of the perfluorinated cationic precursor unlocks the path toward a vast variety of polyfluorinated trityl radicals.
KW - Dye
KW - Fluorescence
KW - Radical
KW - Synthesis
KW - Mechanism
KW - Signal enhancement
KW - Nano
KW - Particle
KW - Characterization
KW - Quantum yield
KW - Photophysics
KW - Lifetime
KW - Polarity
KW - Polymer
KW - Solvatchromism
KW - Excimer
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647973
DO - https://doi.org/10.1021/jacs.5c16418
SN - 0002-7863
VL - 147
IS - 46
SP - 1
EP - 8
PB - American Chemical Society (ACS)
AN - OPUS4-64797
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sommerfeld, Thomas
A1 - Riedel, Juliane
A1 - Lisec, Jan
A1 - Mauch, Tatjana
A1 - Richter, Silke
A1 - Koch, Matthias
T1 - Development of a certified reference material for per- and polyfluoroalkyl substances (PFAS) in textiles
N2 - Per- and polyfluoroalkyl substances (PFASs) are a large group of emerging organic pollutants that contaminate the environment, food, and consumer products. Textiles and other outdoor products are a major source of PFAS exposure due to their water-repellent impregnations. Determination of PFASs in textiles is increasingly important for enhancing their contribution to the circular economy. While maximum levels and restrictions exist for certain key compounds under the Stockholm Convention on Persistent Organic Pollutants and the REACH regulation, certified reference materials (CRMs) are not currently available. To address this issue, the first CRM for determining PFASs in outdoor textiles (BAM-B003) was developed. It fully complies with the requirements of ISO 17034 and ISO 33405. This work presents the entire process of CRM development process, including preparation, a homogeneity study, a stability study, and value assignment. Certification was based on an in-house study at BAM using liquid chromatography tandem mass spectrometry (LC–MS/MS) with stable isotope dilution analysis (SIDA). The certified mass fractions of 18 PFASs range widely from 0.46 to 69 µg/kg, with a prevalence of PFOA (69 µg/kg), PFOS (41 µg/kg) and PFHxA (35 µg/kg) exceeding legal limits. BAM-B003 is intended for analytical quality control and contributes to improving the chemical safety of textiles and strengthening the circular economy.
KW - Reference Material
KW - PFAS
KW - Textiles
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641040
DO - https://doi.org/10.1007/s00216-025-06098-2
SN - 1618-2642
SP - 1
EP - 9
PB - Springer Science and Business Media LLC
AN - OPUS4-64104
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Osiopova, Viktoriia
A1 - Tavernaro, Isabella
A1 - Ge, L.
A1 - Kitzmann, W. R.
A1 - Heinze, K.
A1 - Reithofer, M. R.
A1 - Resch-Genger, Ute
T1 - Complete protection of NIR-luminescent molecular rubies from oxygen quenching in air by L-arginine-mediated silica nanoparticles
N2 - The application of emerging luminophores such as near-infrared (NIR) emissive complexes based on earth-abundant chromium as central ion and triplet-triplet annihilation upconversion (TTA-UC) systems in air as optical reporters for bioimaging or photonic materials for energy conversion requires simple and efficient strategies for their complete protection from uminescence quenching by oxygen. Therefore, we explored the influence of sol–gel synthesis routes on the oxygen protection efficiency of the resulting core and core/shell silica nanoparticles (SiO2 NPs), utilizing the molecular ruby-type luminophores CrPF6 ([Cr(ddpd)2](PF6)3; ddpd = N,N'-dimethyl-N,N'-dipyridin-2-ylpyridin-2,6-diamine) and CrBF4 ([Cr(ddpd)2](BF4)3) with their oxygendependent, but polarity-, proticity-, viscosity-, and concentration-independent luminescence as optical probes for oxygen permeability. The sol–gel chemistry routes we assessed include the classical Stöber method and the underexplored Larginine approach, which relies on the controlled hydrolysis of tetraethoxysilane (TEOS) in a biphasic cyclohexane/water system with the catalyst L-arginine. As demonstrated by luminescence measurements of air- and argon-saturated dispersions of CrPF6- and CrBF4-stained SiO2 NPs of different size and particle architecture, utilizing the luminescence decay kinetics of argon-saturated solutions of CrPF6 and CrBF4 in acetonitrile (ACN) as benchmarks, only SiO2 NPs or shells synthesized by the L-arginine approach provided complete oxygen protection of the CrIII complexes under ambient conditions. We ascribe the different oxygen shielding efficiencies of the silica networks explored to differences in density and surface chemistry of the resulting nanomaterials and coatings, leading to different oxygen permeabilities. Our Larginine based silica encapsulation strategy can open the door for the efficient usage of oxygen-sensitive luminophores and TTA-UC systems as optical reporters and spectral shifters in air in the future.
KW - Quality assurance
KW - Fluorescence
KW - Quantification
KW - Advanced materials
KW - Nano
KW - Quantum yield
KW - NIR
KW - Characterization
KW - Electron microscopy
KW - Silica
KW - Synthesis
KW - Oxygen sensing
KW - Surface
KW - Doping
KW - Lifetime
KW - Cr(III) complex
KW - Shielding
KW - Sensing
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638271
DO - https://doi.org/10.26599/NR.2025.94907241
SN - 1998-0000
VL - 18
IS - 3
SP - 1
EP - 13
PB - SciOpen
AN - OPUS4-63827
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Soyka, J. P.
A1 - Witte, J. F.
A1 - Wiesner, A.
A1 - Krappe, A. R.
A1 - Wehner, D.
A1 - Alnicola, N.
A1 - Paulus, B.
A1 - Resch-Genger, Ute
A1 - Eigler, S.
T1 - [3]Radialene Fluorophores with pH-Switchable Emission and Stable Absorption Maxima
N2 - The first push–pull quino [3]radialene fluorescent dye is reported. Herein, the novel bis(dicyanomethylene)-[3]radialene electron acceptor is connected to a benzimidazole donor. With protonation, a substantial redshift of fluorescence wavelength is observed, while the absorption maximum remains stable. This process is accompanied with an increased fluorescence quantum yield to about 70%. Further, the findings are explained by a combined experimental and theoretical approach, and it is found that vibronic coupling plays a crucial role. This study highlights the yet unexplored potential of [3]radialene-based motifs for the design of environment-responsive fluorophores.
KW - DADQ
KW - Nanographene
KW - fluorescence
KW - Nano
KW - Particle
KW - Synthesis
KW - Characterization
KW - Advanced material
KW - Quantum yield
KW - Photophysic
KW - pH
KW - Probe
KW - Sensor
KW - Lifetime
KW - Polarity
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642147
DO - https://doi.org/10.1002/ejoc.202500669
SN - 1099-0690
SP - 1
EP - 6
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-64214
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hartmann, Yannic
A1 - El Abbassi, Abdelouahad
A1 - Mayer, Bernhard
A1 - Resch-Genger, Ute
A1 - Müller, Thomas J. J.
T1 - Ester‐Aroyl‐S,N‐Ketene Acetals with Solid‐State Luminescence: AIEgens from Sequential Three‐Component Desymmetrization
N2 - AbstractDi(hetero)aroyl dichlorides are desymmetrized upon sequential reaction with alcohols and 2‐methyl N‐benzyl thiazolium salts within the course of a one‐pot three‐component reaction yielding ester‐substituted aroyl‐S,N‐ketene acetals under mild conditions in good yields. A prerequisite for the concise one‐pot process is the different nucleophilicity of the alcohols and in situ generated S,N‐ketene acetals. The resulting compounds are merocyanines with dominant charge‐transfer absorption bands which are fluorescent in the solid state, but not in solution. In water/ethanol solvent mixtures of increasing water content, the water‐insoluble dyes display typical aggregation‐induced emission (AIE) characteristics. The water fraction inducing AIE as well as the emission color, and fluorescence quantum yield (Φf) of the aggregated dyes can be controlled by the alcohol part of the ester moiety. Encapsulation into polystyrene nanoparticles can lead to a considerable increase of the fluorescence quantum yield Φf to 30% as shown for a representatively chosen dye revealing the highest Φf of 11% within the dye series in the water/ethanol mixtures and enabling the usage of these dyes as fluorescent reporters in aqueous environments.
KW - Dye
KW - Fluorescence
KW - Aggregation
KW - Mechanism
KW - Signal enhancement
KW - Nano
KW - Particle
KW - Characterization
KW - Quantum yield
KW - Photophysics
KW - Probe
KW - Sensor
KW - Lifetime
KW - Polarity
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642400
DO - https://doi.org/10.1002/chem.202502071
SN - 0947-6539
SP - 1
EP - 10
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-64240
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Nowatzky, Yannek
A1 - Russo, Francesco Friedrich
A1 - Lisec, Jan
A1 - Kister, Alexander
A1 - Reinert, Knut
A1 - Muth, Thilo
A1 - Benner, Philipp
T1 - FIORA: Local neighborhood-based prediction of compound mass spectra from single fragmentation events
N2 - Non-targeted metabolomics holds great promise for advancing precision medicine and biomarker discovery. However, identifying compounds from tandem mass spectra remains a challenging task due to the incomplete nature of spectral reference libraries. Augmenting these libraries with simulated mass spectra can provide the necessary references to resolve unmatched spectra, but generating high-quality data is difficult. In this study, we present FIORA, an open-source graph neural network designed to simulate tandem mass spectra. Our main contribution lies in utilizing the molecular neighborhood of bonds to learn breaking patterns and derive fragment ion probabilities. FIORA not only surpasses state-of-the-art fragmentation algorithms, ICEBERG and CFM-ID, in prediction quality, but also facilitates the prediction of additional features, such as retention time and collision cross section. Utilizing GPU acceleration, FIORA enables rapid validation of putative compound annotations and large-scale expansion of spectral reference libraries with high-quality predictions.
KW - Metabolomics
KW - Machine Learning
KW - Mass spectrometry
KW - Bioinformatics
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627585
DO - https://doi.org/10.1038/s41467-025-57422-4
SN - 2041-1723
VL - 16
IS - 1
SP - 1
EP - 17
PB - Springer Science and Business Media LLC
AN - OPUS4-62758
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - López-Puertollano, Daniel
A1 - Duncan, Hadyn
A1 - Abad-Somovilla, Antonio
A1 - Abad-Fuentes, Antonio
A1 - Rurack, Knut
T1 - Competitive cytometry-based immunoassay for patulin determination in apple juice
N2 - Patulin is a mycotoxin that is frequently found in apples and apple-derived products. Given the potential harm it can cause to humans, maximum levels for patulin in food have been set worldwide. Conventional methods for the detection of patulin are often time-consuming or lack sensitivity. In this study, a novel cytometry approach based on specific monoclonal antibodies is presented. These high-affinity binders do not target patulin itself, but a stable derivative (adduct) that is rapidly obtained in an aqueous medium at room temperature. To develop the assay, a specific fluorescent competitor was designed and synthesized. After optimizing the assay conditions, including the concentration of the fluorescent competitor and of the antibody bound to polystyrene-silica core–shell microparticles, a detection limit of 0.03 μg L-1 in buffer was achieved. Finally, validation according to Commission Regulation (EU) 2023/2782 demonstrated that apple juice samples spiked with patulin at 25 or 50 μg L-1 (permissible limits set by the EU) were properly scored as non-compliant without any additional treatment other than a simple dilution step in buffer. The developed assay offers several key advantages, including rapid analysis, high sensitivity and specificity, and the potential for multiplexing, making it a promising analytical tool for routine monitoring of patulin contamination in food.
KW - Bead-based assay
KW - Cytometry
KW - Derivatization
KW - Mycotoxin
KW - Patulin
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627659
DO - https://doi.org/10.1016/j.microc.2025.113287
SN - 1095-9149
VL - 212
SP - 1
EP - 8
PB - Elsevier B.V.
AN - OPUS4-62765
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - López-Puertollano, Daniel
A1 - Tobias, Charlie
A1 - Bell, Jérémy
A1 - Abad-Somovilla, A.
A1 - Abad-Fuentes, A.
A1 - Rurack, Knut
T1 - Superparamagnetic Bead-Based Microfluidic Fluoroimmunoassay Platform for Rapid Ochratoxin A Detection in Flour
N2 - Simplification and reduction of time and costs are the primary goals in the development and use of onsite methods in diagnostics and food safety. To facilitate the transition from laboratory techniques to simple, miniaturized devices, we have developed a modular microfluidic platform. This platform integrates a competitive fluorescence immunoassay on the surface of superparamagnetic beads, serving as a complementary technique to traditional cytometry assays. In the first chip module, a fast competitive reaction (5 min) occurs, after which the particles are retained in the second module. This module consists of a PDMS chip and a permanent magnet, allowing only the fluorescent competitor to reach the detection module. Ochratoxin A (OTA) was chosen as the model analyte for device development, using fluorescein-labeled OTA as a competitor. The system efficiently separates particles, with OTA concentration directly correlated to the amount of fluorescent competitor remaining in solution after the competitive reaction. This innovative setup allows to perform rapid measurements with small sample volumes in a short time (10 min), achieving a limit of detection for OTA of 1.2 μg L–1. The system was successfully applied to the accurate determination of OTA in wheat flour spiked at regulatorily relevant concentrations. Using this device, conventional cytometry immunoassays can be seamlessly transformed into user-friendly, miniaturized analytical methods at reduced cost for applications outside of a laboratory directly at the point of need.
KW - Bead-based assay
KW - Fluorescence
KW - Immunoassay
KW - Microfluidics
KW - mycotoxins
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638472
DO - https://doi.org/10.1021/acssensors.5c01119
SN - 2379-3694
SP - 1
EP - 10
PB - American Chemical Society
CY - Washington, D.C.
AN - OPUS4-63847
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Abram, Sarah-Luise
A1 - Tavernaro, Isabella
A1 - Resch-Genger, Ute
A1 - Johnston, L. J.
A1 - Zou, S.
T1 - Nanoscale reference and test materials for the validation of characterization methods for engineered nanomaterials — current state, limitations, and needs
N2 - The rational design of engineered nanomaterials (NMs) with improved functionality and their increasing industrial application requires reliable, validated, and ultimately standardized characterization methods for their application-relevant, physicochemical key properties such as size, size distribution, shape, or surface chemistry. This calls for nanoscale (certified)
reference materials (CRMs; RMs) and well-characterized reference test materials (RTMs) termed also quality control (QC) samples, assessed, e.g., in interlaboratory comparisons, for the validation and standardization of commonly used characterization methods. Thereby, increasing concerns regarding potential risks of NMs are also addressed and the road for safe and
sustainable-by-design concepts for the development of new functional NMs and their use as nanomedicines is paved. With this respect, we will provide an overview of relevant international standardization and regulatory activities, definitions, and recommendations on characterization methods and review currently available organic or inorganic nanoscale CRMs, RMs, and RTMs, including their characterization or certification. In addition, we will highlight typical applications to streamline the regulatory approval process and improve manufacturability including the special challenges imposed by the colloidal nature and sometimes limited stability of NMs. Subsequently, we will critically assess the limitations of currently available nanoscale RMs and RTMs and address the gaps to be filled in the future such as the availability of NMs that come with reference data on properties other than commonly addressed particle size, such as surface chemistry or particle number concentration, or
more closely resemble commercially available formulations or address application-relevant matrices.
KW - Nano
KW - Particle
KW - Silica
KW - Quality assurance
KW - Reference material
KW - Review
KW - Surface chemistry
KW - Size
KW - Shape
KW - Particle number concentration
KW - Lipid nanoparticles
KW - Metal nanoparticles
KW - Liposomes
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625746
DO - https://doi.org/10.1007/s00216-024-05719-6
SN - 1618-2650
SP - 1
EP - 21
PB - Springer
AN - OPUS4-62574
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tavernaro, Isabella
A1 - Sander, P. C.
A1 - Andresen, Elina
A1 - Schedler, U.
A1 - Resch-Genger, Ute
T1 - Expanding the Toolbox of Simple, Cost-Efficient, and Automatable Methods for Quantifying Surface Functional Groups on Nanoparticles� Potentiometric Titration
N2 - Measuring surface functional groups (FGs) on nanomaterials (NMs) is essential for designing dispersible and stable NMs with tailored and predictable functionality. FG screening and quantification also plays a critical role for subsequent processing steps, NM long-term stability, quality control of NM production, and risk assessment studies and enables the implementation of sustainable and safe(r)-by-design concepts. This calls for simple and cost-efficient methods for broadly utilized FGs that can be ideally automated to speed up FG screening, monitoring, and quantification. To expand our NM surface analysis toolbox, focusing on simple methods and broadly available, cost-efficient instrumentation, we explored a NM-adapted pH titration method with potentiometric and optical readout for measuring the total number of (de)protonable FGs on representatively chosen commercial and custom-made aminated silica nanoparticles (SiO2 NPs). The accuracy and robustness of our stepwise optimized workflows was assessed by several operators in two laboratories and method validation was done by cross-comparison with two analytical methods relying on different signal generation principles. This included traceable, chemo-selective quantitative nuclear magnetic resonance spectroscopy (qNMR) and thermogravimetric analysis (TGA), providing the amounts of amino silanes released by particle dissolution and the total mass of the surface coatings. A comparison of the potentiometric titration results with the reporter-specific amounts of surface amino FGs determined with the previously automated fluorescamine (Fluram) assay highlights the importance of determining both quantities for surface-functionalized NMs. In the future, combined NM surface analysis with optical assays and pH titration will simplify quality control of NM production processes and stability studies and can yield large data sets for NM grouping that facilitates further developments in regulation and standardization.
KW - Quality assurance
KW - Fluorescence
KW - Nano
KW - Particle
KW - Synthesis
KW - Characterization
KW - Advanced material
KW - Surface
KW - Standardization
KW - Reference material
KW - Functional group
KW - Quantification
KW - Coating
KW - Automation
KW - Potentiometry
KW - Method
KW - Validation
KW - Optical assay
KW - Fluram
KW - Fluorescamine
KW - qNMR
KW - Comparison
KW - ILC
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642371
DO - https://doi.org/10.1021/acsmeasuresciau.5c00062
SN - 2694-250X
SP - 1
EP - 13
PB - American Chemical Society
CY - Washington, DC
AN - OPUS4-64237
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Herter, Sven-Oliver
A1 - Haase, Hajo
A1 - Koch, Matthias
T1 - Semisynthesis of Stable Isotope-Labeled Ergot Alkaloids for HPLC-MS/MS Analysis
N2 - Ergot alkaloids (EAs) are prevalent food contaminants affecting cereals, such as rye, wheat, and barley worldwide. To ensure EU safety standards, the six most common EAs: ergometrine, ergotamine, ergosine, ergocornine, ergocristine, and ergocryptine, and their epimers, are quantified using HPLC-MS/MS, as described in the European Standard Method EN 17425:2021. However, this can be challenging and time-consuming in food matrices without appropriate internal standards and highlights the need for more robust and precise analytical tools to support their monitoring. The development of isotope-labeled EAs directly addresses this gap, offering improved accuracy and leading to more consistency across laboratories and consequently to more consumer safety. Therefore, we developed a semisynthetic approach, building upon our previous work where native ergotamine was N6-demethylated to norergotamine and subsequently remethylated using iodomethane (13CD3-I). Herein, we are now able to present the successful synthesis of all of the isotopically labeled priority EAs. These isotope-labeled standards were tested against their native counterparts using HPLC coupled with HR-MS/MS. The chromatographic and mass spectrometric properties of the unlabeled and isotopically labeled EAs match exactly, confirming their successful synthesis and structure. These standards can now be utilized to enhance the accuracy and reliability of EA quantification in food and feed.
KW - Reference Material
KW - HPLC-MS/MS
KW - Mycotoxins
KW - Ergot Alkaloids
KW - Stable Isotope Dilution Analysis
KW - Semisynthesis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639692
DO - https://doi.org/10.1021/acs.jafc.5c03345
SN - 0021-8561
VL - 73
IS - 29
SP - 18412
EP - 18419
PB - American Chemical Society (ACS)
AN - OPUS4-63969
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stiegler, L. M. S.
A1 - Wegner, Karl David
A1 - Weigert, Florian
A1 - Peukert, W.
A1 - Resch-Genger, Ute
A1 - Walter, J.
T1 - Analysis of Giant-Shell CdSe/CdS Quantum Dots via Analytical Ultracentrifugation Combined with Spectrally Resolved Photoluminescence
N2 - Knowledge of the structure–property relationships of functional nanomaterials, including, for example, their size- and composition-dependent photoluminescence (PL) and particle-to-particle variations, is crucial for their design and reproducibility. Herein, the Angstrom-resolution capability of an analytical ultracentrifuge combined with an in-line multiwavelength emission detection system (MWE-AUC) for measuring the sedimentation coefficient-resolved spectrally corrected PL spectra of dispersed nanoparticles is demonstrated. The capabilities of this technique are shown for giant-shell CdSe/CdS quantum dots (g-QDs) with a PL quantum yield (PL QY) close to unity capped with oleic acid and oleylamine ligands. The MWE-AUC PL measurements are calibrated and validated with certified fluorescence standards. The spectrally corrected and size-dependent PL spectra of the g-QDs derived from a single MWE-AUC experiment are then analyzed and compared with the results of single-particle spectroscopic studies, yielding the PL spectra, decay kinetics, and blinking behavior of individual g-QDs. This study underlines the vast potential of MWE-AUC with in-line optical detection for the characterization of advanced nanomaterials with a complex structure.
KW - Quantum dots
KW - Analytical ultracentrifugation
KW - Photoluminescence
KW - Advanced nanomaterial characterization
KW - Calibrated fluorescence measurements
KW - Reference materials
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624357
DO - https://doi.org/10.1002/smtd.202401700
SN - 2366-9608
SP - 1
EP - 7
PB - Wiley VHC-Verlag
AN - OPUS4-62435
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Richter, Maria
A1 - Güttler, Arne
A1 - Pauli, Jutta
A1 - Vogel, K.
A1 - Homann, Christian
A1 - Würth, Christian
A1 - Resch-Genger, Ute
T1 - Extending certified spectral fluorescence standards for the calibration and performance validation of fluorescence instruments to the NIR—closing the gap from 750 to 940 nm with two novel NIR dyes
N2 - Fluorescence techniques such as fluorescence spectroscopy, microfluorometry, and fluorescence microscopy, providing spectral, intensity, polarization, and lifetime information, are amongst the most broadly utilized analytical methods in the life and materials sciences. However, the measured fluorescence data contain sample- and instrument-specific contributions, which hamper their comparability across instruments and laboratories. Comparable, instrument-independent fluorescence data require the determination of the fluorescence instrument’s wavelength-dependent spectral responsivity, also termed emission correction curve, for the same instrument settings as those used for the fluorescence measurements as a prerequisite for the subsequent correction of the measured instrument-specific data. Such a spectral correction is essential for the performance comparison of different fluorescent labels and reporters, quantitative fluorescence measurements, the determination of the fluorescence quantum yield, and the spectroscopic measure for the fluorescence efficiency of a fluorophore. Simple-to-use tools for obtaining emission correction curves are chromophore-based reference materials (RMs), referred to as fluorescence standards, with precisely known, preferably certified instrument-independent fluorescence spectra. However, for the increasingly used near-infrared (NIR) wavelength region >700 nm, at present, no spectral fluorescence standards are available. To close this gap, we developed two novel spectral fluorescence standards, BAM F007 and BAM-F009, with broad emission bands from about 580 to 940 nm in ethanolic solution. These liquid fluorescence standards currently under certification, which will be released in 2025, will expand the wavelength range of the already available certified Calibration Kit BAM F001b-F005b from about 300–730 to 940 nm. In this research article, we will detail the criteria utilized for dye and matrix selection and the homogeneity and stability tests accompanying dye certification as well as the calculation of the wavelength-dependent uncertainty budgets of the emission spectra BAM F007 and BAM-F009, determined with the traceably calibrated BAM reference spectrofluorometer. These fluorescence standards can provide the basis for comparable fluorescence measurements in the ultraviolet, visible, and NIR for the fluorescence community.
KW - Quality assurance
KW - Reference material
KW - Fluorescence
KW - Dye
KW - Traceability
KW - Metrology
KW - Calibration
KW - Reference data
KW - Reference product
KW - Digital certificate
KW - NIR
KW - Instrument performance validation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626317
DO - https://doi.org/10.1007/s00216-024-05723-w
SN - 1618-2650
SP - 1
EP - 15
PB - Springer
AN - OPUS4-62631
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Krappe, Alexander R.
A1 - Mayer, Jacob C.
A1 - Zhang, Wuai
A1 - Filla, Lina M.
A1 - Ligorio, Giovanni
A1 - Hermerschmidt, Felix
A1 - Eitelhuber, Larissa S.
A1 - Güttler, Arne
A1 - Weber, Manuela
A1 - Paulus, Beate
A1 - Resch-Genger, Ute
A1 - List-Kratochvil, Emil J.W.
A1 - Eigler, Siegfried
T1 - Highly Emissive Hexa-peri-benzocoronene-fluoranthene Hybrid as Easily Processable and Stable OLED Material
N2 - We report the synthesis of a fluorescent polycyclic aromatic hydrocarbon dye with a “symmetry-broken” core, derived from the related hexa-peri-benzocoronene (HBC) core with fluoranthene subunit. The fluorophore is composed of a pure Carbon skeleton without heteroatoms and exhibits remarkable photo luminescence properties with a photoluminescence Quantum yield (PLQY) of up to 67% in toluene, exceeding that of theparent HBC by a factor of 30. The single crystal X-ray structure reveals the distorted polycyclic aromatic hydrocarbon structure, which is responsible for the optoelectronic properties, as supported by density functional theory calculations. We show that the new fluorescent dye can be readily used for the fabrication of organic light-emitting diodes (OLED) without extensive optimization, whereby solubility in a variety of solvents and successful film formation are decisive.
KW - Quantum Yield
KW - OLED
KW - Fluorescence
KW - Synthesis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631298
DO - https://doi.org/10.1002/chem.202500742
SN - 1521-3765
SP - 1
EP - 7
PB - John Wiley & Sons, Inc
AN - OPUS4-63129
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Frenzel, F.
A1 - Fiedler, S.
A1 - Bardan, A.
A1 - Güttler, Arne
A1 - Würth, Christian
A1 - Resch-Genger, Ute
T1 - Influence of Measurement Geometry and Blank on Absolute Measurements of Photoluminescence Quantum Yields of Scattering Luminescent Films
N2 - For a series of 500 μm-thick polyurethane films containing different concentrations of luminescent and scattering YAG:Ce microparticles, we systematically explored and quantified pitfalls of absolute measurements of photoluminescence quantum yields (Φf) for often employed integrating sphere (IS) geometries, where the sample is placed either on a sample holder at the bottom of the IS surface or mounted in the IS center. Thereby, the influence of detection and illumination geometry and sample position was examined using blanks with various scattering properties for measuring the number of photons absorbed by the sample. Our results reveal that (i) setup configurations where the scattering sample is mounted in the IS center and (ii) transparent blanks can introduce systematic errors in absolute Φf measurements.
For strongly scattering, luminescent samples, this can result in either an under- or overestimation of the absorbed photon flux and hence an under- or overestimation of Φf. The size of these uncertainties depends on the scattering properties of the sample and instrument parameters, such as sample position, IS size, wavelength-dependent reflectivity of the IS surface coating, and port configuration. For accurate and reliable absolute Φf measurements, we recommend (i) a blank with scattering properties closely matching those of the sample to realize similar distributions of the diffusely scattered excitation photons within the IS, and (ii) a sufficiently high sample absorption at the excitation wavelength. For IS setups with center-mounted samples, measurement geometries should be utilized that prevent the loss of excitation photons by reflections from the sample out of the IS.
KW - Quality assurance
KW - Fluorescence
KW - Nano
KW - Particle
KW - Quantum yield
KW - Characterization
KW - Silica
KW - Scattering
KW - Uncertainty
KW - Film
KW - Pphosphor
KW - YAG:Ce
KW - LED
KW - Converter material
KW - Solid material
KW - Polymer
KW - Composite material
KW - Advanced material
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638304
DO - https://doi.org/10.1021/acs.analchem.4c06726
SN - 1520-6882
SP - 1
EP - 8
PB - ACS Publications
AN - OPUS4-63830
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tavernaro, Isabella
A1 - Simon, Fabian
A1 - Gehrenkemper, Lennart
A1 - Tobias, Charlie
A1 - Resch-Genger, Ute
A1 - Meermann, Björn
T1 - Quantification of the amount of surface groups of aminated silica nano- and microparticles utilizing a fluorine tag and HR-CS-GFMAS
N2 - The performance, bioavailability, and safe use of engineered nanomaterials (NMs) depends not only on properties such as size, shape, and surface area, but largely on surface chemistry. While many sizing methods have been established, there is still a lack of validated screening methods for determining NM surface functional groups (FGs). In this context, we present a fast and simple method for FG quantification using high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) and assess its applicability for the surface analysis of representatively chosen aminated silica nanoparticles (NPs) and microparticles (MPs) in conjunction with amino FG labeling with a fluorine tag. For this proof-of-concept study, first surface amino FG screening of the silica NPs and MPs was done with a potentiometric back titration method, providing the total amount of protonatable surface FGs, and two optical assays relying on reporter dyes with sizes and spatial requirements, i.e., surface binding areas smaller or larger than that of the fluorine tag to estimate the maximum and reporter-accessible number of amino FGs. Subsequently, the surface amino FGs were labeled with the fluorine tag 4-(trifluoromethyl)benzoic acid (TFMB) and the amount of fluorine originating from the bound TFMB molecules was quantified by HR-CS-GFMAS in two common organic solvents, i.e., dimethyl sulfoxide (DMSO) or ethanol (EtOH) to assess possible interferences from organic matrices. Our study revealed limits of detection (LODs) and quantification (LOQs) for fluorine of 1.0 µg/L and 3.5 µg/L in EtOH and 1.5 µg/L and 5.0 µg/L in DMSO, respectively. Overall, a quick and simple method for analyzing surface FGs on NPs and MPs was presented utilizing broadly available fluorine tags and HR-CS-GFMAS for fluorine quantification, which can be applied, e.g., for homogeneity, stability, and aging studies of surface-modified particles. This could contribute to ease the understanding of property-safety relationships for surface-functionalized NMs.
KW - Fluorine Analysis
KW - Nano- and microparticles
KW - Surface group quantification
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641965
DO - https://doi.org/10.1007/s00216-025-06107-4
SN - 1618-2642
SP - 1
EP - 11
PB - Springer Science and Business Media LLC
CY - Berlin ; Heidelberg
AN - OPUS4-64196
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scharek, Vera M.
A1 - Kröger, Tommy
A1 - Keil, Karin
A1 - Traub, Heike
A1 - Meermann, Björn
T1 - A new elemental analytical approach for microplastic sum parameter analysis—ETV/ICP-MS with CO2
N2 - Microplastics (MPs) are pervasive environmental pollutants and are considered one of the main challenges of our time. However, a fast and comprehensive analytical approach for MP analysis in complex matrices traceable to SI units is still lacking. In this context, we report a fast screening tool for the sum parameter analysis of MPs using electrothermal vaporization (ETV) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). In our proof-of-concept study, we observed size-independent detection of MPs as peaks above the 13C+ signal background in the nano- to micrometer range without limitations regarding the polymer type. Quantification of the 13C+ MP signals was accomplished via an external gas calibration utilizing dynamic dilution of carbon dioxide with argon, yielding recovery rates of 80–96% for MP reference material (RM) of polymer types commonly found in the environment. The applicability to a soil sample was demonstrated through spiking experiments with a polyethylene (PE) MP RM in soil. The limit of detection (LOD) was estimated to be 0.13 µg C, equaling the detection of a single spherical low-density-PE particle of about 70 µm, and a limit of quantification (LOQ) of 0.42 µg C.
KW - ETV/ICP-MS
KW - Mikroplastik
KW - Summenparameter
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646418
DO - https://doi.org/10.1007/s00216-025-06146-x
SN - 1618-2642
SP - 1
EP - 10
PB - Springer
CY - Berlin ; Heidelberg
AN - OPUS4-64641
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Bayerl, C.
A1 - Shahryari, M.
A1 - Reiter, R.
A1 - Proß, V.
A1 - Lehmann, K.
A1 - Kühl, A. A.
A1 - Becker, Dorit
A1 - Schulz, Andreas
A1 - Infante Duarte, C.
A1 - Taupitz, M.
A1 - Geisel, D.
A1 - Tzschätzsch, H.
A1 - Saatz, Jessica
A1 - Traub, Heike
A1 - Asbach, P.
T1 - Quantitative Analysis of Gadolinium Deposits in Liver Tissue of Patients After Single or Multiple Gadolinium-based Contrast Agent Application
N2 - Gadolinium-based contrast agents (GBCAs) are widely used in magnetic resonance imaging. Concerns exist regarding gadolinium deposition and its potential histopathologic tissue alterations, especially after repeated administrations of linear, less stable GBCAs. This study aimed to quantify gadolinium mass fractions in liver specimens of subjects exposed to GBCAs in correlation with histopathologic features.
In this study, mass fractions of gadolinium in human liver specimens from 25 subjects who underwent liver tumor resection surgery and had received GBCA (1 to 9 times over 4 years), were quantitatively analyzed using inductively coupled plasma–mass spectrometry (ICP-MS). Histomorphology was assessed based on the nonalcoholic fatty liver disease activity score (NAS).
Our results suggest that after intravenous administration of GBCA, a small fraction of gadolinium is retained in the liver over a time period of at least several weeks. A relationship was observed between Gadolinium retention and the number of GBCA administrations, but not with the cumulative dose and the degree of fatty liver disease.
KW - ICP-MS
KW - Contrast agent
KW - Gadolinium
KW - Liver
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646608
DO - https://doi.org/10.1097/RLI.0000000000001254
SN - 1536-0210
SP - 1
EP - 10
PB - Lippincott Williams & Wilkins
CY - Philadelphia, Pa.
AN - OPUS4-64660
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lozano-Martín, Daniel
A1 - Tuma, Dirk
A1 - Chamorro, César R.
T1 - Evaluation of Reference Equations of State for Density Prediction in Regasified LNG Mixtures Using High-Precision Experimental Data
N2 - This study evaluates the performance of three reference equations of state (EoS), AGA8-DC92, GERG-2008, and SGERG-88, in predicting the density of regasified liquefied natural gas (RLNG) mixtures. A synthetic nine-component RLNG mixture was gravimetrically prepared. High-precision density measurements were obtained using a single-sinker magnetic suspension densimeter over a temperature range of (250 to 350) K and pressures up to 20 MPa. The experimental data were compared with EoS predictions to evaluate their accuracy. AGA8-DC92 and GERG-2008 showed excellent agreement with the experimental data, with deviations within their stated uncertainty. In contrast, SGERG-88 exhibited significantly larger deviations for this RLNG mixture, particularly at low temperatures of (250 to 260) K, where discrepancies reached up to 3 %. Even at 300 K, deviations larger than 0.4 % were observed at high pressures, within the model’s uncertainty, but notably higher than those of the other two EoSs. The analysis was extended to three conventional 11-component natural gas mixtures (labeled G420 NG, G431 NG, and G432 NG), previously studied by our group using the same methodology. While SGERG-88 showed reduced accuracy for the RLNG mixture, it performed reasonably well for these three mixtures, despite two of them have a very similar composition to the RLNG. This discrepancy is attributed to the lower CO2 and N2 content typical in RLNG mixtures, demonstrating the sensitivity of EoS performance to minor differences in composition. These findings highlight the importance of selecting appropriate EoS models for accurate density prediction in RLNG applications.
KW - Regasified LNG
KW - Equation of state
KW - Density
KW - Gravimetric preparation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646506
DO - https://doi.org/10.1007/s10765-025-03669-4
SN - 0195-928X
VL - 46
SP - 1
EP - 25
PB - Springer Science and Business Media LLC
CY - Heidelberg
AN - OPUS4-64650
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heide, Maximilian
A1 - Reifenrath, Jonas
A1 - Herrmann, Alexander
A1 - Engelhard, Carsten
T1 - Fast and Sustainable Active Pharmaceutical Ingredient (API) Screening in Over-the-Counter and Prescription Drug Products by Surface-Assisted Plasma-Based Desorption/Ionization High-Resolution Mass Spectrometry
N2 - Fast chemical analysis of pharmaceutical preparations is important for quality assurance, counterfeit drug detection, and consumer health. While quantitative methods such as high-performance liquid chromatography mass spectrometry (HPLC-MS) are powerful, there is a need for sustainable and environmentally friendly methods, which require less chemicals and produce less waste. Here, solvent-free ambient desorption/ionization (ADI) MS methods are attractive because they do not require time-consuming chromatography, produce little to no chemical waste, and, thus, contribute to green chemistry practice. In addition, sample throughput can be higher compared to HPLC-MS. In this study, a method for direct analysis of single- and multi agent drugs using a plasma-based ADI source (flowing atmospheric-pressure afterglow, FAPA) coupled to high-resolution (HR) MS was developed and optimized for best performance. The approach is rapid and only requires analytes to be in solution (only a few µL) before application onto thin-layer chromatography (TLC) surfaces, specifically dimethyl (RP2-) and cyano (CN-) modified silica, for surface-assisted (SA) FAPA-HRMS measurements. No chromatographic separation was required, and the TLC plates served only as sample carriers. A broad variety of 19 active pharmaceutical ingredients (APIs) was carefully selected to cover analgesics, anesthetics, antibiotics, antiepileptics, calcium channel blockers, diuretics, expectorants, opioids, peripheral vasodilators, stimulants, and sympathomimetics. Fast screening and identification of APIs was performed by SA-FAPA-HRMS. Typically, the protonated molecular ion ([M+H]+) was the most abundant species, while some compounds (codeine, metamizole, phenoxymethylpenicillin, and torasemide) did show some degree of fragmentation. As a proof-of-principle application, benzocaine was directly detected in saliva samples post-intake of a lozenge. Time-resolved semi-quantitative screening was performed. The limit of detection for benzocaine in saliva was 8 ng/mL (48.4 fmol) using internal standard calibration and CN-HPTLC plates. In addition, direct quantification of artificially spiked saliva was performed with minimal sample preparation. Here, SA-FAPA-HRMS with a CN-HPTLC sample substrate yielded best performance (20.02±0.52 µg/mL, RSD=2.6%, deviation of -1.9% from the theoretical value) compared to RP2-TLC (18.97±1.37 µg/mL, RSD=7.2%, -7.0%), and HPLC-UV (18.51±0.03 µg/mL, RSD=0.2%, -9.3%) results. In conclusion, SA FAPA HRMS is considered attractive for rapid and sustainable analysis of pharmaceuticals with potential in non-invasive patient monitoring.
KW - Mass Spectrometry
KW - Pharmaceuticals
KW - Green Chemistry
KW - Ambient Desorption/Ionization
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640718
DO - https://doi.org/10.1039/D5AY01050K
SN - 1759-9660
VL - 17
IS - 18
SP - 7799
EP - 7809
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64071
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Homann, Christian
A1 - Peeters, Régis
A1 - Mirmajidi, Hana
A1 - Berg, Jessica
A1 - Fay, Michael
A1 - Rodrigues, Lucas Carvalho Veloso
A1 - Radicchi, Eros
A1 - Jain, Akhil
A1 - Speghini, Adolfo
A1 - Hemmer, Eva
T1 - Rapid microwave-assisted synthesis of morphology-controlled luminescent lanthanide-doped Gd2O2S nanostructures
N2 - Gadolinium oxysulfide (Gd2O2S) is an attractive material of demonstrated suitability for a variety of imaging applications, leveraging its magnetic, scintillating, and luminescent properties, particularly when doped with optically active lanthanide ions (Ln3+). For many of these applications, control over size and morphology at the nanoscale is crucial. This study demonstrates the rapid microwave-assisted Synthesis of colloidal Ln2O2S (Ln = Gd and dopants Yb, Er, Tb) nanostructures in as little as 20 min. Structural characterization using X-ray diffraction analysis (XRD), Raman spectroscopy, as well as Transmission electron microscopy (TEM), including elemental mapping via energy dispersive X-ray spectroscopy (EDS), unveiled the key role of elemental sulphur (S8) in the reaction mixtures for materials growth. By systematically varying the Ln-to-S ratio from 1 : 0.5 to 1 : 15, controlled morphologies ranging from triangular nanoplatelets to berry- and flower-like shapes were achieved. Doping with Er3+/Yb3+ endowed the nano-triangles with upconverting and near-infrared emitting properties. Tb3+-doped Gd2O2S exhibited the characteristic green Tb3+ emission under UV excitation, while also showing X-ray excited optical luminescence (XEOL), rendering the material interesting as a potential nano-scintillator.
KW - Upconversion
KW - Microwave-assisted synthesis
KW - Synthesis
KW - Fluorescence
KW - Nano
KW - Particle
KW - NIR
KW - XRD
KW - X-ray fluoressence
KW - Morphology control
KW - Raman
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647907
DO - https://doi.org/10.1039/D5TC01646K
SN - 2050-7526
VL - 13
IS - 35
SP - 18492
EP - 18507
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64790
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Frenzel, Olivia
A1 - Westphalen, Tanja
A1 - Kaminski, Katja
A1 - Kluge, Stephanie
A1 - Bücker, Michael
A1 - Piechotta, Christian
T1 - Evaluation and Validation of an Accelerated Weathering Procedure to Characterise the Release of Bisphenol A from Polycarbonate Under Exposure to Simulated Environmental Conditions
N2 - Bisphenol A (BPA) has been listed as a substance of very high concern (SVHC) due to its endocrine-disrupting properties according to REACH in 2017. European competent authorities have prepared a REACH restriction proposal to reduce BPA levels in the environment. The proposed limit for the concentration of free BPA and other bisphenols in articles is 10 mg kg−1. If exceeded, migration testing can demonstrate that no more than 0.04 mg L−1 is released from the product or material over its lifetime. German authorities are drafting a new restriction proposal after the original was temporarily withdrawn. The residual and migration limits mentioned above were key requirements from the previous restriction proposal. Numerous national and international standards exist for assessing how environmental factors affect the physical and chemical properties of products and materials—such as notch impact strength and tensile strength—but these standards do not cover the release of pollutants. A standardised procedure that covers all aspects of artificial weathering and monitors the subsequent release of pollutants is necessary, especially in the context of the regulation of these substances. An accelerated weathering procedure was established for non-protected samples. This material was not intended for outdoor applications. The testing procedure applied a typical weathering scenario that represents Central European climate conditions. The procedure was validated and applied to samples under distinct quality assurance aspects. Released BPA is quantified via an organic isotope dilution LC-MS/MS method. In parallel, identical samples were weathered outdoors on a weathering rack. Haze and yellowness index are measured to compare outdoor and weathering chamber results.
KW - Artificial weathering
KW - Polycarbonate
KW - Bisphenol A
KW - Simulated environmental conditions
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645020
DO - https://doi.org/10.3390/app151910361
SN - 2076-3417
VL - 15
IS - 19
SP - 1
EP - 15
PB - MDPI AG
AN - OPUS4-64502
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Matiushkina, Anna
A1 - Abram, Sarah-Luise
A1 - Tavernaro, Isabella
A1 - Richstein, R.
A1 - Reithofer, M. R.
A1 - Andresen, Elina
A1 - Michaelis, Matthias
A1 - Koch, Matthias
A1 - Resch-Genger, Ute
T1 - Quantifying Citrate Surface Ligands on Iron Oxide Nanoparticles with TGA, CHN Analysis, NMR, and RP-HPLC with UV Detection
N2 - Although citrate is frequently used as a surface ligand for nanomaterials (NMs) such as metal, metal oxide, and lanthanide-based NMs in hydrophilic environments due to its biocompatibility and simple replacement by other more strongly binding ligands in postsynthetic surface modification reactions, its quantification on NM surfaces has rarely been addressed. Here, we present a multimethod approach for citrate quantification on iron oxide nanoparticles (IONPs) broadly applied in the life and material sciences. Methods explored include thermogravimetric (TGA) and elemental (CHN) analysis, providing citrate-nonspecific information on the IONP coating, simple photometry, and citrate-selective reversed-phase high-performance liquid chromatography (RP-HPLC) with absorption (UV) detection and quantitative nuclear magnetic resonance spectroscopy (qNMR). Challenges originating from the strongly absorbing magnetic NM and paramagnetic iron species interfering with optical and NMR Methods were overcome by suitable sample preparation workflows. Our multimethod approach to citrate quantification highlights the advantages of combining specific and unspecific methods for characterizing NM Surface chemistry and method cross-validation. It also demonstrates that chemically nonselective measurements can favor an overestimation of the amount of a specific surface ligand by signal contributions from molecules remaining on the NM surface, e.g., from particle synthesis, such as initially employed ligands and/or surfactants. Our results emphasize the potential of underexplored selective RPHPLC for quantifying ligands on NMs, which does not require a multistep sample preparation workflow such as qNMR for many NMs and provides a higher sensitivity. These findings can pave the road to future applications of versatile HPLC methods in NM characterization.
KW - Advanced material
KW - Functional group
KW - Iron oxide
KW - Ligand
KW - Nano
KW - Particle
KW - Quantification
KW - Surface analysis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648632
DO - https://doi.org/10.1021/acs.analchem.5c03024
SN - 0003-2700
VL - 97
IS - 36
SP - 19627
EP - 19634
PB - American Chemical Society (ACS)
CY - Washington, DC
AN - OPUS4-64863
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Jaeger, Carsten
A1 - Lintelmann, Jutta
A1 - Franke, Raimo
A1 - Artati, Anna
A1 - Cecil, Alexander
A1 - Broda, Frank
A1 - Klawonn, Frank
A1 - Erban, Alexander
A1 - Kopka, Joachim
A1 - Fuchs, Beate
A1 - Sommer, Ulf
A1 - Neumann-Schaal, Meina
A1 - O'Connor, Gavin
T1 - Analytical practices, use and needs of standard and reference materials in the German-speaking metabolomics community: results of an online survey
N2 - Introduction
Since the early 2000s, metabolomics has grown rapidly, becoming integral to fields like life sciences, health, and environmental research. This expansion has led to the formation of national and international societies, such as Germany’s DGMet, to tackle emerging challenges. One of DGMet’s goals is to improve measurement quality by assessing community needs for harmonization and standardization. A recent survey within the German-speaking community aimed to identify current practices and gaps in the use of chemical standards and reference materials, to guide future standardization efforts and collaborative initiatives.
Methods
An online survey was conducted between June 2023 and April 2024. The survey consisted of 38 key questions and was open to research institutions from Germany, Austria, and Switzerland.
Results
The survey was accessed by 68 laboratories, with 23 institutes providing complete or partial responses (34% response rate), which is comparable to rates reported in similar surveys within the metabolomics and lipidomics communities. Respondents were mainly experienced researchers from Germany, focusing mainly on health-related (“red”) metabolomics, as indicated by 78% of the respondents, followed by microbial (“grey”, 48%) and plant (“green”, 39%) metabolomics (multiple answers possible). The use of targeted methods was reported more frequently (91%) than that of non-targeted methods (78%), whereas metabolite fractions studied were equally split between polar, midpolar and lipid fractions (83% each). Human (74%), mouse (61%) and Arabidopsis (30%) were the most frequently studied organisms. Most participants used synthetic chemical standards for instrument qualification (83%), calibration (78%), and metabolite identification (74%), while matrix reference materials were mainly applied for quality control (52%) and method validation (44%). There was a strong demand for more standards, especially for metabolite identification and quantification, with cost being a major barrier, particularly for isotopically labelled standards and certified reference materials.
Conclusions
Valuable insights into the use of standards and reference materials within the German-speaking metabolomics community were obtained. Moving forward, the community should address critical gaps in metabolomics standardization. To achieve this, it must share its knowledge, articulate its needs clearly, and actively engage in joint efforts with national metrology institutes and international standardization initiatives.
KW - Reference material
KW - Chemical standard
KW - Metabolomics
KW - Mass spectrometry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647303
DO - https://doi.org/10.1007/s11306-025-02360-x
VL - 21
IS - 6
SP - 1
EP - 11
PB - Springer-Nature
CY - Heidelberg
AN - OPUS4-64730
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Steinbeck, Christoph
A1 - Jung, Nicole
A1 - Bach, Felix
A1 - Neumann, Steffen
A1 - Herres-Pawlis, Sonja
A1 - Liermann, Johannes
A1 - Koepler, Oliver
A1 - Bannwarth, Christoph
A1 - Bender, Theo
A1 - Bocklitz, Thomas
A1 - Boehm, Franziska
A1 - Bonatto Minella, Christian
A1 - Biedermann, Frank
A1 - Brack, Werner
A1 - Cunha, Ricardo
A1 - Czodrowski, Paul
A1 - Eberl, Franziska
A1 - Engel, Thomas
A1 - Engstfeld, Albert
A1 - Fischer, Tillmann G.
A1 - Friedrich, Pascal
A1 - Glorious, Frank
A1 - Golub, Benjamin
A1 - Grathwol, Christoph
A1 - Haag, Rainer
A1 - Hunold, Johannes
A1 - Jacob, Christoph
A1 - Johannsen, Jochen
A1 - Jollife, John
A1 - Kast, Stefan
A1 - Kettner, Carsten
A1 - Kuhn, Stefan
A1 - Lanza, Giacomo
A1 - Lisec, Jan
A1 - Manolikakes, Georg
A1 - Mata, Ricardo
A1 - Meiler, Jens
A1 - Müller, Matthias
A1 - Müller-Pfefferkorn, Ralph
A1 - Ortmeyer, Jochen
A1 - Patterson, Wendy
A1 - Pleiss, Jürgen
A1 - Riedel, Annalisa
A1 - Riedel, Jens
A1 - Schatzschneider, Ulrich
A1 - Schuster, Leonie
A1 - Seeberger, Peter
A1 - Seibert, Johann-Nikolaus
A1 - Stadler, Peter
A1 - Zeitler, Kirsten
T1 - Proposal NFDI4Chem 2025-2030 In the National Research Data Infrastructure (NFDI) — Our Vision: All Chemists Publish FAIR Data
N2 - The first funding period of NFDI4Chem established a robust foundation for research data management (RDM) in chemistry by promoting FAIR data principles and creating a cohesive infrastructure to capture well-annotated data early in the lab through electronic lab notebooks (ELNs) and making this data available in public repositories. Key achievements include standardised data formats and metadata, a federated repository environment, and improved data visibility and accessibility. Training programs and outreach have significantly increased awareness and adoption of best RDM practices. In the second funding period, the consortium aims to advance these achievements by consolidating this infrastructure, developing a model for its sustainable maintenance and operation, and fostering cultural change for its widespread adoption. Goals include ensuring seamless data workflows from laboratories to open repositories, enhancing interoperability, and supporting innovative research through AI-ready data. The work plan is organised into six task areas (TAs). TA1 (Management) provides leadership and supports all other TAs in achieving their objectives. TA2 (Smart Lab) aims to develop a fully digital research environment, including an ELN as a modular platform. This environment will support data collection, management, storage, analysis, and sharing. Integrating devices and external resources will enable seamless data transfer to repositories. TA3 (Repositories) will consolidate the repository ecosystem. The goal is to integrate repositories into a federated system for better accessibility and interoperability, ensuring long-term data availability and sustainability. TA4 (Metadata, Data Standards, and Publication Standards) focuses on developing and promoting new data and metadata standards in an international community process. This includes applying ontologies to create a semantic foundation for linking research data, making it machine-readable and enabling knowledge graphs. TA5 (Community and Training) is dedicated to fostering a cultural shift towards digital chemistry through continuous engagement, collecting requirements, and providing extensive training and support through workshops and open education resources. It will promote FAIR-compliant machine learning applications, embedding RDM into academic curricula to ensure future scientists are well-versed in these practices. TA6 (Synergies and Cross-Cutting Topics) aims to enhance collaboration across NFDI consortia and beyond. This includes developing ontologies, terminology services, the search service, and other cross-cutting solutions, integrating these developments into existing infrastructure, enabling interdisciplinary data harmonisation and fostering machine learning applications.
KW - Research Data Management
KW - FAIR
KW - Chemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648540
DO - https://doi.org/10.3897/rio.11.e177037
SN - 2367-7163
VL - 11
SP - 1
EP - 100
PB - Pensoft Publishers
AN - OPUS4-64854
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Li, Xunyu
A1 - Riedel, Jens
A1 - You, Yi
T1 - Spectrally resolved lithium isotope quantification through high-resolution spatial heterodyne spectrometry
N2 - Isotope ratio determination of lithium is increasingly important in fields ranging from geochemistry to battery diagnostics. While mass spectrometry remains the gold standard, it is costly, cumbersome, and incompatible with portable or inline implementations. Optical emission spectroscopy presents an appealing alternative. However, it is traditionally limited by insufficient spectral resolution or resolving power to separate lithium isotope emissions due to their generalized designs for a wide spectral range; this often requires overly complicated algorithms to overcome the instrumental drawbacks. (79)
Results Here, we report a high-resolution optical method for lithium isotope quantification using a custom-built spatial heterodyne spectrometer (SHS) combined with a reduced-pressure glow discharge source. This configuration yielded a resolving power of 189,000 and enabled baseline resolution of lithium d-line emission features even without the need for preliminary data processing. Despite the inherent low sensitivity of SHS, a detection limit of 30 pmol was achieved using a standard industrial camera. To improve quantitative accuracy, we introduced a deconvolution-based spectral lineshape recovery technique alongside a bootstrapping-based error propagation strategy. These methods facilitated robust isotope ratio calibration using both peak-height and peak-area metrics. The SHS platform additionally enabled the determination of relative transition probabilities, suggesting the feasibility of calibration-free operation.
This work demonstrates the practical viability of SHS for high-specificity, high-resolution lithium isotope analysis. The approach is compact, potentially field-deployable, and adaptable to other elements with optically resolvable isotope shifts, offering a route toward accessible and calibration-free optical isotopic analyses.
KW - SHS
KW - Isotope
KW - High-resolution spectroscopy
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635139
DO - https://doi.org/10.1016/j.aca.2025.344329
SN - 1873-4324
VL - 1368
SP - 1
EP - 8
PB - Elsevier B.V.
AN - OPUS4-63513
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mohan, M.
A1 - Prochazka, D.
A1 - You, Yi
A1 - Riedel, Jens
A1 - Gornushkin, Igor
A1 - Rocnakova, I.
A1 - Papula, M.
A1 - Porízka, P.
A1 - Kaizer, J.
T1 - Investigating plasma morphology at material boundaries under varying ambient pressures
N2 - Laser-Induced Breakdown Spectroscopy (LIBS) is a widely used technique for elemental analysis. The analysis of the obtained LIBS spectra generally assumes plasma homogeneity. However, using focused laser beams for interrogation, LIBS probes materials on the microscale and is, thus, prone to artefacts from sample heterogeneities on the micrometer scale. An ablation at a material boundary of two matrices may result in a significant inhomogeneity in the plasma plume, which can severely impact the accuracy of quantitative analysis. Since this propagation of the surface morphology into the plasma plume is driven by the plasma expansion, its final impact is strongly pressure dependent. This study examines the influence of varying ambient pressures (7–1000 mbar) on plasma morphology, spectral characteristics, and key plasma properties such as electron number density at a well-defined Cu–Sn boundary, in comparison with the results obtained using homogeneous alloys. Several approaches of plasma imaging with bandpass filters, spectroscopy, and Radon transform-based 3D reconstruction were employed to analyze elemental distribution, signal-to-noise (SNR) and signal-to-background (SBR) ratios, as well as electron number densities. The 3D reconstructions revealed a pronounced plasma asymmetry for the ablation at the material boundary, in contrast to the near-axial symmetry observed for the ablation of homogeneous alloys. At lower pressures, this distinct elemental separation in plasma persisted, while higher pressures led to an increased collisional mixing and homogenization. SNR and SBR were consistently lower for ablation at the boundary compared to homogeneous samples. These findings highlight how boundary ablation contributes to plasma inhomogeneities in LIBS analysis of heterogeneous materials and emphasize the need to account for these
effects when using LIBS for elemental mapping of fine heterogeneous structures.
KW - Laser-induced breakdown spectroscopy
KW - Plasma inhomogeneity
KW - Plasma tomography
KW - Radon transform
KW - Material boundaries
KW - Ambient pressure effects
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634777
DO - https://doi.org/10.1016/j.talanta.2025.128377
SN - 1873-3573
VL - 295
SP - 1
EP - 8
PB - Elsevier B.V.
AN - OPUS4-63477
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kleinbub, Sherin
A1 - Braymer, Joseph J
A1 - Pfeiffer, Friedhelm
A1 - Dyall-Smith, Mike
A1 - Spirgath, Kristin
A1 - Alfaro-Espinoza, Gabriela
A1 - Koerdt, Andrea
T1 - From Genes to Black Rust: Genomic insights into corrosive methanogens
N2 - Within the past ten years, genetic evidence has been increasing for the direct role that microbes play in microbiologically influenced corrosion (MIC), also known as biocorrosion or biodeterioration. One prominent example is the correlation between the corrosion of metal and the presence of genes encoding an extracellular [NiFe]-hydrogenase (MIC hydrogenase) in the methanogenic archaeon, Methanococcus maripaludis. In this study, DNA sequencing and bioinformatic analysis were used to classify the MIC hydrogenase as belonging to a core set of genes, the MIC core, found so far in Methanococci and Methanobacteria classes of methanogens. Genetic evidence is provided for the mobilization of the MIC core via multiple mechanisms, including a horizontal gene transfer event from Methanobacteria to Methanococci and a newly described MIC-transposon. A detailed comparison of M. maripaludis genomes further pointed to the relevance that cell wall modifications involving N-glycosylation of S-layer proteins and the MIC hydrogenase likely play in methanogen-induced MIC (Mi-MIC). Microscopic analysis of corrosive methanogens encoding the MIC core indicated that Methanobacterium-affiliated strain IM1 can form extensive biofilms on the surface of corrosion products whereas individual cells of M. maripaludis Mic1c10 were only found localized to crevices in the corrosion layer. An updated model of Mi-MIC involving two modes of action is presented, which predicts that the propensity of cells to adhere to iron surfaces directly influences the rate of corrosion due to the localization of the MIC hydrogenase at the metal-microbe interface.
KW - Biocorrosion
KW - Hydrogenases
KW - Metalloprotein
KW - Microbes
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649425
DO - https://doi.org/10.1093/femsmc/xtaf018
SN - 2633-6685
VL - 6
SP - 1
EP - 19
PB - Oxford University Press (OUP)
AN - OPUS4-64942
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Richter, Matthias
A1 - Schühle, Florian
T1 - Experimental determination of 7-day uptake rates for diffusive sampling of 86 volatile and semi-volatile organic compounds relevant for indoor air monitoring and investigation on their sensitivity to exposure time and indoor climate
N2 - This study aimed to experimentally determine uptake rates for 86 indoor relevant volatile and semi-volatile organic compounds (VOC, SVOC) for the passive sampler type Perkin Elmer/Markes™ with Tenax® TA as sorbent, which was used in the German Environmental Survey on Health (GerES VI) carried out by the German Environmental Agency (UBA) in the years 2023-2024. For this purpose, single reference gas atmospheres of 76 pure VOCs (liquid at room temperature) and a group of 10 SVOCs and VOCs (solid at room temperature) were generated using two generation procedures. By exposing the samplers to individual components, it was ruled out that interactions in a mixture have a influence on the uptake rate. Another aspect was to precisely describe the methodology and the resulting uncertainties, as there are gaps in the literature in this regard. The selection of the compounds was based on the findings of the preceding GerES V study for which data was missing or needed to be verified. In each experiment, a number of six passive samplers was exposed to the test gas atmospheres in dynamically operated exposure chambers for seven days. The sensitivity of the uptake rates of a group of 10 selected VOCs to variations in exposure time, ambient temperature, and air humidity in a multi-component reference gas atmosphere was investigated. Here, a decrease in the uptake rate with the exposure time could be observed stabilising from the fifth day of exposure onwards. A significant effect of temperature and humidity on the uptake rate was not apparent. The determined uptake rates exhibit uncertainties of < 20 % for 71 substances, and < 10 % for 51 substances which are also in good agreement with the literature, if already published elsewhere. The quantity of investigated substances, the detailed description of the methodology used to determine the uptake rates complemented by the respective uncertainties, as well as the compilation of comparative data, contribute to a better assessment of the quality and relevance of such data, which had not been published before.
KW - Indoor air quality
KW - Volatile organic compounds
KW - Uptake rates
KW - Passive sampling
KW - Tenax TA
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629913
DO - https://doi.org/10.1016/j.indenv.2025.100095
VL - 2
IS - 2
SP - 1
EP - 11
PB - Elsevier
AN - OPUS4-62991
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sun, Yijuan
A1 - Pérez-Padilla, Víctor
A1 - Valderrey, Virginia
A1 - Bell, Jérémy
A1 - Gawlitza, Kornelia
A1 - Rurack, Knut
T1 - Ratiometric detection of perfluoroalkyl carboxylic acids using dual fluorescent nanoparticles and a miniaturised microfluidic platform
N2 - The widespread contamination of soil and water with perfluoroalkyl substances (PFAS) has caused considerable societal and scientific concern. Legislative measures and an increased need for remediation require effective on-site analytical methods for PFAS management. Here we report on the development of a green-fluorescent guanidine-BODIPY indicator monomer incorporated into a molecularly imprinted polymer (MIP) for the selective detection of perfluorooctanoic acid (PFOA). Complexation of PFOA by the indicator, which is mediated by concerted protonation-induced ion pairing-assisted hydrogen bonding, significantly enhances fluorescence in polar organic solvents. The MIP forms as a thin layer on silica nanoparticles doped with tris(bipyridine)ruthenium(II) chloride, which provides an orange emission signal as internal reference, resulting in low measurement uncertainties. Using a liquid-liquid extraction protocol, this assay enables the direct detection of PFOA in environmental water samples and achieves a detection limit of 0.11 µM. Integration into an opto-microfluidic system enables a compact and user-friendly system for detecting PFOA in less than 15 minutes.
KW - PFAS
KW - Molecular imprinting
KW - Microfluidics
KW - Fluorescence
KW - Onsite assay
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650270
DO - https://doi.org/10.1038/s41467-025-66872-9
SN - 2041-1723
VL - 16
IS - 1
SP - 1
EP - 16
PB - Springer Science and Business Media LLC
AN - OPUS4-65027
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Oskoei, Párástu
A1 - Afonso, Rúben
A1 - Bastos, Verónica
A1 - Nogueira, João
A1 - Keller, Lisa-Marie
A1 - Andresen, Elina
A1 - Saleh, Maysoon I.
A1 - Rühle, Bastian
A1 - Resch-Genger, Ute
A1 - Daniel-da-Silva, Ana L.
A1 - Oliveira, Helena
T1 - Upconversion Nanoparticles with Mesoporous Silica Coatings for Doxorubicin Targeted Delivery to Melanoma Cells
N2 - Melanoma is one of the most aggressive skin cancers and requires innovative therapeutic strategies to overcome the limitations of conventional therapies. In this work, upconversion nanoparticles coated with mesoporous silica and functionalized with folic acid (UCNP@mSiO2-FA) were developed as a targeted nanocarrier system for the delivery of doxorubicin (DOX). The UCNPs were synthesized via thermal decomposition, coated with mesoporous silica shells, and functionalized with folic acid (FA) to enable receptor-mediated targeting. DOX was then loaded into the mesoporous silica coating by adsorption, yielding UCNP@mSiO2-FA-DOX. The different UCNPs were characterized for size, composition, colloidal stability, and loading and release of DOX. This comprehensive physicochemical characterization confirmed a high DOX loading efficiency and a slightly increased drug release under acidic conditions, mimicking the tumour microenvironment. In vitro assays using four melanoma cell lines (A375, B16-F10, MNT-1, and SK-MEL-28) revealed an excellent biocompatibility of UCNP@mSiO2-FA and a significantly higher cytotoxicity of UCNP@mSiO2-FA-DOX compared to unloaded UCNPs, in a dose-dependent manner. Cell cycle analysis demonstrated G2/M phase arrest after treatment with UCNP@mSiO2-FA-DOX, confirming its antiproliferative effect. Overall, UCNP@mSiO2-FA-DOX represents a promising nanoplatform for targeted melanoma therapy, combining active tumour targeting and enhanced anticancer efficacy.
KW - Fluorescence
KW - Synthesis
KW - Nano
KW - Particle
KW - Silica
KW - Cell
KW - Uptake
KW - Drug
KW - Characterization
KW - DOX
KW - Imaging
KW - Toxicity
KW - Release
KW - pH
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653596
DO - https://doi.org/10.3390/molecules31010074
SN - 1420-3049
VL - 31
IS - 1
SP - 1
EP - 18
PB - MDPI AG
AN - OPUS4-65359
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ahmed, A. A. A.
A1 - Alegret, N.
A1 - Almeida, B.
A1 - Alvarez-Puebla, R.
A1 - Andrews, A. M.
A1 - Ballerini, L.
A1 - Barrios-Capuchino, J. J.
A1 - Becker, C.
A1 - Blick, R. H.
A1 - Bonakdar, S.
A1 - Chakraborty, I.
A1 - Chen, X.
A1 - Cheon, J.
A1 - Chilla, G.
A1 - Conceicao, A. L. C.
A1 - Delehanty, J.
A1 - Dulle, M.
A1 - Efros, A. L.
A1 - Epple, M.
A1 - Fedyk, M.
A1 - Feliu, N.
A1 - Feng, M.
A1 - Fernandez-Chacon, R.
A1 - Fernandez-Cuesta, I.
A1 - Fertig, N.
A1 - Förster, S.
A1 - Garrido, J. A.
A1 - George, M.
A1 - Guse, A. H.
A1 - Hampp, N.
A1 - Harberts, J.
A1 - Han, J.
A1 - Heekeren, H. R.
A1 - Hofmann, U. G.
A1 - Holzapfel, M.
A1 - Hosseinkazemi, H.
A1 - Huang, Y.
A1 - Huber, P.
A1 - Hyeon, T.
A1 - Ingebrandt, S.
A1 - Ienca, M.
A1 - Iske, A.
A1 - Kang, Y.
A1 - Kasieczka, G.
A1 - Kim, D.-H.
A1 - Kostarelos, K.
A1 - Lee, J.-H.
A1 - Lin, K.-W.
A1 - Liu, S.
A1 - Liu, X.
A1 - Liu, Y.
A1 - Lohr, C.
A1 - Mailänder, V.
A1 - Maffongelli, L.
A1 - Megahed, S.
A1 - Mews, A.
A1 - Mutas, M.
A1 - Nack, L.
A1 - Nakatsuka, N.
A1 - Oertner, T. G.
A1 - Offenhäusser, A.
A1 - Oheim, M.
A1 - Otange, B.
A1 - Otto, F.
A1 - Patrono, E.
A1 - Peng, B.
A1 - Picchiotti, A.
A1 - Pierini, F.
A1 - Pötter-Nerger, M.
A1 - Pozzi, M.
A1 - Pralle, A.
A1 - Prato, M.
A1 - Qi, B.
A1 - Ramos-Cabrer, P.
A1 - Resch-Genger, Ute
A1 - Ritter, N.
A1 - Rittner, M.
A1 - Roy, S.
A1 - Santoro, F.
A1 - Schuck, N. W.
A1 - Schulz, F.
A1 - Seker, E.
A1 - Skiba, M.
A1 - Sosniok, M.
A1 - Stephan, H.
A1 - Wang, R.
A1 - Wang, T.
A1 - Wegner, Karl David
A1 - Weiss, P. S.
A1 - Xu, M.
A1 - Yang, C.
A1 - Zargarin, S. S.
A1 - Zeng, Y.
A1 - Zhou, Y.
A1 - Zhu, D.
A1 - Zierold, R.
A1 - Parak, W. J.
T1 - Interfacing with the Brain: How Nanotechnology Can Contribute
N2 - Interfacing artificial devices with the human brain is the central goal of neurotechnology. Yet, our imaginations are often limited by currently available paradigms and technologies. Suggestions for brain−machine interfaces have changed over time, along with the available technology.
Mechanical levers and cable winches were used to move parts of the brain during the mechanical age. Sophisticated electronic wiring and remote control have arisen during the electronic age, ultimately leading to plug-and-play computer interfaces. Nonetheless, our brains are so complex that these visions, until recently, largely remained unreachable dreams. The general problem, thus far, is that most of our technology is mechanically and/or electrically engineered, whereas the brain is a living, dynamic entity. As a result, these worlds are difficult to interface with one another. Nanotechnology, which encompasses engineered solid-state objects and integrated circuits, excels at small length scales of single to a few hundred nanometers and, thus, matches the sizes of biomolecules, biomolecular assemblies, and parts of cells. Consequently, we envision nanomaterials and nanotools as opportunities to interface with the brain in alternative ways. Here, we review the existing literature on the use of nanotechnology in brain−machine interfaces and look forward in discussing perspectives and limitations based on the authors’ expertise across a range of complementary disciplines from neuroscience, engineering, physics, and chemistry to biology and medicine, computer science and mathematics, and social science and jurisprudence. We focus on nanotechnology but also include information from related fields when useful and complementary.
KW - Nanoneuro interface
KW - Brain-on-a-chip
KW - Nanostructured interface
KW - Electrode arrays
KW - Neuro-implants
KW - Advanced nanomaterials
KW - Quality assurance
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634893
DO - https://doi.org/10.1021/acsnano.4c10525
SN - 1936-086X
VL - 19
IS - 11
SP - 10630
EP - 10717
PB - ACS Publications
AN - OPUS4-63489
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
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 - 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 - 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 - 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 - Obenlüneschloß, Jorit
A1 - Boysen, Nils
A1 - Rönnby, Karl
A1 - Muriqi, Arbresha
A1 - Hoffmann, Volker
A1 - Abad Andrade, Carlos Enrique
A1 - Rogalla, Detlef
A1 - Brokmann, Ulrike
A1 - Rädlein, Edda
A1 - Nolan, Michael
A1 - Devi, Anjana
T1 - Ein seltener mononuklearer Lithium‐Carben‐Komplex für die Atomlagenabscheidung von lithiumhaltigen Dünnschichten
N2 - KurzfassungLithium ist das zentrale Element moderner Batterietechnologien, und die Herstellung von lithiumhaltigen Materialien mittels Atomlagenabscheidung (engl. Atomic Layer Deposition, ALD) bietet erhebliche Vorteile bei der Kontrolle der Schichtdicke und ‐zusammensetzung. In dieser Studie wird ein neuer mononuklearer, durch ein N‐heterocyclisches Carben (NHC) stabilisierter Lithiumkomplex, [Li(tBuNHC)(hmds)], als vielversprechender Präkursor für die ALD von lithiumhaltigen Dünnschichten vorgestellt. Die strukturelle Charakterisierung erfolgt durch den Vergleich von Dichtefunktionaltheorie (DFT) und Einkristall‐Röntgenbeugung (engl. Single‐Crystal X‐ray Diffraction, SC‐XRD), wobei die seltene mononukleare Struktur bestätigt wird. Thermogravimetrische Analysen (TGA) zeigen vorteilhafte thermische Eigenschaften für ALD‐Anwendungen. Die Verbindung weist einen niedrigen Schmelzpunkt, saubere Verdampfung und ermutigende Volatilitätsparameter im Vergleich zu anderen Lithium‐Präkursoren auf. ALD‐Experimente mit [Li(tBuNHC)(hmds)] und Ozon zeigen dessen Effektivität bei der Abscheidung von LiSixOy‐Filmen. Der ALD‐Prozess zeigt ein gesättigtes Wachstum pro Zyklus (engl. Growth per Cycle, GPC) von 0,95 Å. Die Zusammensetzung, analysiert mittels Rutherford‐Rückstreu‐Spektrometrie/Kernreaktionsanalyse (engl. Rutherford Backscattering Spectrometry/Nuclear Reaction Analysis, RBS/NRA), Röntgenphotoelektronenspektroskopie (engl. X‐ray Photoelectron Spectroscopy, XPS) und Glimmentladungsspektroskopie (engl. Glow Discharge Optical Emission Spectrometry, GD‐OES), bestätigt das Vorhandensein von Lithium und Silizium in den erwarteten Verhältnissen. Diese Arbeit stellt nicht nur einen neuen ALD‐Präkursor vor, sondern trägt auch zum Verständnis der Lithiumchemie bei und bietet Einblicke in die faszinierende Koordinationschemie und das thermische Verhalten von durch NHC‐Liganden stabilisierten Lithiumkomplexen.
KW - Atomlagenabscheidung
KW - N-heterozyklischer-Carben-(NHC)-stabilisierter Lithium-Präkursor
KW - Mononuklearer Li–Carben-Komplex
KW - Lithiumsilicat-Dünnfilme
KW - Filmanalytik/-Charakterisierung
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644045
DO - https://doi.org/10.1002/ange.202513066
SN - 0044-8249
N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier
SP - 1
EP - 12
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-64404
LA - deu
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 - 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 - 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 - 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 - Döring, Sarah
A1 - Tscheuschner, Georg
A1 - Flemig, Sabine
A1 - Weller, Michael G.
A1 - Konthur, Zoltán
T1 - Cost-Effective Method for Full-Length Sequencing of Monoclonal Antibodies from Hybridoma Cells
N2 - Background: Monoclonal antibodies play an important role in therapeutic and analytical applications. For recombinant expression, the coding sequences of the variable regions of the heavy and light chains are required. In addition, cloning antibody sequences, including constant regions, reduces the impact of hybridoma cell loss and ensures preservation of the naturally occurring full antibody sequence. Method: We combined amplification of IgG antibody variable regions from hybridoma mRNA with an advanced method for fulllength cloning of monoclonal antibodies in a simple two-step workflow. Following Sanger sequencing and evaluation of consensus sequences, the best matching variable, diversity,
and joining (V-(D-)J) gene segments were identified according to identity scores from IgBLAST reference sequences. Simultaneously, the mouse IgG subclass was determined at the DNA level based on isotype-specific sequence patterns in the CH1 domain. Knowing the DNA sequence of V-(D-)J recombination responsible for the complementary determining region 3 (CDR 3), variable region-specific primers were designed and used to amplify the corresponding antibody constant regions. Results: To verify the approach, we applied it to the hybridoma clone BAM-CCMV-29-81 and obtained identical full-length antibody
sequences as with RNA Illumina sequencing. Further validation at the protein level using an established MALDI-TOF MS-fingerprinting protocol showed that five out of six genetically encoded CDR domains of the monoclonal antibody BAM-CCMV-29-81 could be efficiently correlated. Conclusion: This simple, streamlined method enables the cost-effective determination of the full-length sequence of monoclonal antibodies from hybridoma cell lines, with the added benefit of obtaining the DNA sequence of the antibody ready for recombinant expression.
KW - Full-length antibody sequencing
KW - Hybridoma cell loss
KW - MALDI-TOF MS
KW - Immunoglobulin isotyping
KW - RNA Illumina sequencing
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639599
DO - https://doi.org/10.3390/antib14030072
SN - 2073-4468
VL - 14
IS - 3
SP - 1
EP - 17
PB - MDPI
CY - Basel
AN - OPUS4-63959
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Döring, Sarah
T1 - Corundum Particles as Trypsin Carrier for Efficient Protein Digestion
N2 - This dataset contains raw LC–MS/MS files of trypsin-digested NISTmAb acquired on a SCIEX TripleTOF 6600 mass spectrometer in DIA (SWATH) mode for antibody quantification. In addition, it includes MALDI-TOF MS peptide mass fingerprints of trypsin-digested Herceptin as well as reference spectra that can be used for antibody identification using the open-source software ABID 2.0 (https://bam.de/ABID).
The data were generated within a study demonstrating the applicability of corundum-immobilized trypsin for antibody digestion and its suitability for peptide-based LC–MS/MS quantification and MALDI-TOF MS fingerprinting–based antibody identification.
KW - NISTmAb
KW - Herceptin
KW - MALDI-TOF MS peptide mass fingerprint
KW - ABID 2.0
PY - 2025
DO - https://doi.org/10.5281/zenodo.17416536
PB - Zenodo
CY - Geneva
AN - OPUS4-65365
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Starkholm, A.
A1 - Al-Sabbagh, Dominik
A1 - Sarisozen, S
A1 - von Reppert, A
A1 - Rössle, M
A1 - Ostermann, Markus
A1 - Unger, E
A1 - Emmerling, Franziska
A1 - Kloo, L
A1 - Svensson, P
A1 - Lang, F
A1 - Maslyanchuk, O.
T1 - Green Fabrication of Sulfonium-Containing Bismuth Materials for High-Sensitivity X-Ray Detection
N2 - Organic–inorganic hybrid materials based on lead and bismuth have recently been proposed as novel X- and gamma-ray detectors for medical imaging, non-destructive testing, and security, due to their high atomic numbers and facile preparation compared to traditional materials like amorphous selenium and Cd(Zn)Te. However, challenges related to device operation, excessively high dark currents, and long-term stability have delayed commercialization. Here, two novel semiconductors incorporating stable sulfonium cations are presented, [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5, synthesized via solvent-free ball milling and fabricated into dense polycrystalline pellets using cold isostatic compression, two techniques that can easily be upscaled, for X-ray detection application. The fabricated detectors exhibit exceptional sensitivities (14 100–15 190 µC Gyair−1 cm−2) and low detection limits (90 nGyair s−1 for [(CH3CH2)3S]6Bi8I30 and 78 nGyair s−1 for [(CH3CH2)3S]AgBiI5), far surpassing current commercial detectors. Notably, they maintain performance after 9 months of ambient storage. The findings highlight [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5 as scalable, cost-effective and highly stable alternatives to traditional semiconductor materials, offering great potential as X-ray detectors in medical and security applications.
KW - Mechanochemistry
KW - X-ray detectors
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630306
DO - https://doi.org/10.1002/adma.202418626
SP - 1
EP - 10
PB - Wiley VHC-Verlag
AN - OPUS4-63030
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Temgoua, Ranil C.T.
A1 - Dontsi, Fabiola T.
A1 - Lebègue, Estelle
A1 - Thobie-Gautier, Christine
A1 - Tonlé, Ignas K.
A1 - Boujtita, Mohammed
T1 - Understanding the behavior of phenylurazole-tyrosine-click electrochemical reaction using hybrid electroanalytical techniques
N2 - In this work, the electrochemical behavior of 4-phenylurazole (Ph-Ur) was studied and the latter was used as a molecular anchor for the electrochemical bioconjugation of tyrosine (Y). Cyclic voltammetry (CV) and controlled potential coulometry (CPC) allowed the in-situ generation of the PTAD (4-phenyl-3 H-1,2,4-triazole-3,5(4 H)-dione) species from phenylurazole on demand for tyrosine electrolabeling. The chemoselectivity of the reaction was studied with another amino acid (lysine, Lys) and no changes in Lys were observed. To evaluate the performance of tyrosine electrolabeling, coulometric analyses at controlled potentials were performed on solutions of phenylurazole and the phenylurazole-tyrosine mixture in different proportions (2:1, 1:1, and 1:2). The electrolysis of the phenylurazole-tyrosine mixture in the ratio (1:2) produced a charge of 2.07 C, very close to the theoretical value (1.93 C), with high reaction kinetics, a result obtained here for the first time. The products obtained were identified and characterized by liquid chromatography coupled to high-resolution electrospray ionization mass spectrometry (LC-HRMS and LC- HRMS2). Two products were formed from the click reactions, one of which was the majority. Another part of this work was to study the electrochemical degradation of the molecular anchor 4-phenylazole (Ph-Ur). Four stable degradation products of phenylurazole were identified (C7H9N2O, C6H8N, C6H8NO, C14H13N4O2) based on chromatographic profiles and mass spectrometry results. The charge generated during the electrolysis of phenylurazole (two-electron process) (2.85 C) is inconsistent with the theoretical or calculated charge (1.93 C), indicating that secondary/parasitic reactions occurred during the electrolysis of the latter. In conclusion, the electrochemically promoted click phenylurazole-tyrosine reactions give rise to click products with high reaction kinetics and yields in the (1:2) phenylurazole-tyrosine ratios, and the presence of side reactions is likely to affect the yield of the click phenylurazole-tyrosine reaction.
KW - Clinical Biochemistry
KW - Spectroscopy
KW - Drug Discovery
KW - Pharmaceutical Science
KW - Analytical Chemistry
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599267
DO - https://doi.org/10.1016/j.jpba.2024.116147
VL - 245
SP - 1
EP - 8
PB - Elsevier BV
AN - OPUS4-59926
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - von Törne, Wipert Jannik
A1 - Steinhäuser, Lorin
A1 - Klyk-Seitz, Urszula-Anna
A1 - Piechotta, Christian
T1 - High-resolution mass spectrometric elucidation of electron ionization induced fragmentation pathways of methylated warfarin and selected hydroxylated species
N2 - The plant secondary metabolite families of coumarin and 4-hydroxy coumarin have a broad pharmacological spectrum ranging from antibacterial to anticancer properties. One prominent member of this substance class is the synthetic but naturally inspired anticoagulant drug and rodenticide warfarin (coumadin). A vast number of publications focus on the identification of warfarin and its major cytochrome P450-mediated phase I metabolites by liquid chromatography (LC) with mass spectrometry (MS) and tandem mass spectrometric (MS/MS) detection techniques. For the first time, electron ionization (EI) induced high-resolution quadrupole time-of-flight mass spectrometric (HR-qToF-MS) data of in-liner derivatized warfarin and selected hydroxylated species is provided in this study as an alternative to LC-MS/MS approaches. Furthermore, the characteristic fragments and fragmentation pathways of the analyzed methyl ethers are concluded. The obtained data of analytical standards, specific deuterated and 13C-labeled compounds prove inductive cleavage of the acyl or acetonyl side chain, methyl migration, and H-migration, along with consequential inductive cleavage as predominant fragmentation routes. Based on the HR-spectral data, commonalities and differences between the analyzed compounds and fragment groups were evaluated with future applicability in structure elucidation and spectra prediction of related compounds.
KW - High-resolution mass spectrometry
KW - Warfarin
KW - Hydroxy warfarin
KW - Fragmentation pathway
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596025
DO - https://doi.org/10.1016/j.ijms.2024.117220
SN - 1387-3806
VL - 499
SP - 1
EP - 7
PB - Elsevier B.V.
AN - OPUS4-59602
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - von Törne, Wipert Jannik
A1 - Klyk-Seitz, Urszula-Anna
A1 - Piechotta, Christian
T1 - Developing a GC-EI-MS/MS method for quantifying warfarin and five hydroxylated metabolites generated by the Fenton reaction
N2 - AbstractSince the 1950s, Warfarin has been used globally as both a prescription drug and a rodenticide. Research has shown that warfarin and other rodenticides are present in the environment and food chain. However, emerging contaminants are subject to degradation by biotic and abiotic processes and advanced oxidation processes. In some cases, detecting the parent compound may not be possible due to the formation of structurally changed species. This approach aims to identify hydroxylated transformation products of warfarin in a laboratory setting, even after the parent compound has undergone degradation. Therefore, the Fenton reaction is utilized to insert hydroxylation into the parent compound, warfarin, by hydroxyl and hydroperoxyl radicals generated by Fe2+/Fe3+ redox reaction with hydrogen peroxide. Using multiple reaction monitoring, a GC–MS/MS method, incorporating isotopically labeled reference compounds, is used to quantify the expected derivatized species. The analytes are derivatized using trimethyl-3-trifluoromethyl phenyl ammonium hydroxide, and the derivatization yield of warfarin is determined by using isotopically labeled reference compounds. The method has a linear working range of 30 to 1800 ng/mL, with detection limits ranging from 18.7 to 67.0 ng/mL. The analytes are enriched using a C18-SPE step, and the recovery for each compound is calculated. The Fenton reaction generates all preselected hydroxylated transformation products of warfarin. The method successfully identifies that 4′-Me-O-WAR forms preferentially under the specified experimental conditions. By further optimizing the SPE clean-up procedures, this GC–MS-based method will be suitable for detecting transformation products in more complex matrices, such as environmental water samples. Overall, this study provides a better understanding of warfarin’s degradation and offers a robust analytical tool for investigating its transformation products.
KW - Health, Toxicology and Mutagenesis
KW - Pollution
KW - Environmental Chemistry
KW - General Medicine
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595737
DO - https://doi.org/10.1007/s11356-024-32133-3
SN - 0944-1344
VL - 31
SP - 16986
EP - 16994
PB - Springer Science and Business Media LLC
AN - OPUS4-59573
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kornev, Roman
A1 - Gornushkin, Igor B.
A1 - Shabarova, Lubov
A1 - Kadomtseva, Alena
A1 - Mochalov, Georgy
A1 - Rekunov, Nikita
A1 - Romanov, Sergey
A1 - Medov, Vitaly
A1 - Belousova, Darya
A1 - Maleev, Nikita
T1 - Plasma-Chemical Disposal of Silicon and Germanium Tetrachlorides Waste by Hydrogen Reduction
N2 - The processes of hydrogen reduction of silicon and germanium chlorides under the conditions of high-frequency (40.68 MHz) counteracted arc discharge stabilized between two rod electrodes are investigated. The main gas-phase and solid products of plasma-chemical transformations are determined. Thermodynamic analysis of SiCl4 + H2 and GeCl4 + H2 systems for optimal process parameters was carried out. Using the example of hydrogen reduction of SiCl4 by the method of numerical modeling, gas-dynamic and thermal processes for this type of discharge are investigated. The impurity composition of gas-phase and solid reaction products is investigated. The possibility of single-stage production of high-purity Si and Ge mainly in the form of compact ingots, as well as high-purity chlorosilanes and trichlorogermane, is shown.
KW - High-frequency arc discharge
KW - Hydrogen reduction
KW - Silicon chlorides
KW - Germanium chlorides
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594454
DO - https://doi.org/10.3390/sci6010001
VL - 6
IS - 1
SP - 1
EP - 12
PB - MDPI AG
AN - OPUS4-59445
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Flierl, Lukas
A1 - Rienitz, Olaf
A1 - Vogl, Jochen
A1 - Pramann, Axel
T1 - An advancement of the gravimetric isotope mixture method rendering the knowledge of the spike purity superfluous
N2 - The gravimetric isotope mixture method is the primary method to determine absolute isotope ratios. This method, however, depends on the existence of suitable spike materials and knowledge of their purities. Determining the purity of the spikes can be tedious and labour-intensive. In this publication, an advancement of the gravimetric isotope mixture method, rendering the determination of the purity of the spike materials unnecessary, is presented. The advancement combines mass spectrometry and ion chromatography leading to an approach being independent of the purity of the spike materials. In the manuscript the mathematical background and the basic idea of the novel approach are described using a two-isotope system like copper or lithium.
KW - Isotope amount ratios
KW - Metrology
KW - Mass spectrometry
KW - Ion chromatography
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608726
DO - https://doi.org/10.1007/s00216-024-05465-9
SP - 5325
EP - 5333
PB - Springer Science and Business Media LLC
AN - OPUS4-60872
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wegner, Karl David
A1 - Hildebrandt, N.
T1 - Near infrared quantum dots for biosensing and bioimaging
N2 - Quantum dots (QDs) possess unique optoelectronic properties, which make them very attractive to be used as optical probes in biosensing and bioimaging applications. The strong absorbance and light scattering of biological compounds like tissue and blood in the visible range pose a problem. However, if optical probes emitting in the near-infrared (NIR) range are used, scattering, absorption, and autofluorescence of biological components are strongly reduced. This allows for an increased light penetration depth and higher spatial and temporal resolution for the investigation of biological processes. The synthesis and application of NIR emitting QDs is a fast-growing research field and the benefits of using QDs were demonstrated for a variety of applications, such as photoelectrochemical biosensor, in vivo vascular imaging, and fluorescence-guided surgery. This article reviews the state-of-the-art developments in the preparation of NIR/IR QDs and highlights the latest research about their utilization in biosensing and bioimaging applications.
KW - Quantum dots
KW - Near-infrared
KW - Biosensing
KW - Bioimaging
KW - NIR-II / SWIR
KW - Advanced nanomaterials
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609708
SN - 0165-9936
DO - https://doi.org/10.1016/j.trac.2024.117922
VL - 180
SP - 1
EP - 19
PB - Elsevier B.V.
AN - OPUS4-60970
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Chronakis, Michail Ioannis
A1 - Meermann, Björn
A1 - von der Au, Marcus
T1 - The evolution of data treatment tools in single-particle and single-cell ICP-MS analytics
N2 - Single-particle inductively coupled plasma-mass spectrometry (sp-ICP-MS) is one of the most powerful tools in the thriving field of nanomaterial analysis. Along the same lines, single-cell ICP-MS (sc-ICP-MS) has become an invaluable tool in the study of the variances of cell populations down to a per-cell basis. Their importance and application fields have been listed numerous times, across various reports and reviews. However, not enough attention has been paid to the immense and ongoing development of the tools that are currently available to the analytical community for the acquisition, and more importantly, the treatment of single-particle and single-cell-related data. Due to the ever-increasing demands of modern research, the efficient and dependable treatment of the data has become more important than ever. In addition, the field of single-particle and single-cell analysis suffers due to a large number of approaches for the generated data—with varying levels of specificity and applicability. As a result, finding the appropriate tool or approach, or even comparing results, can be challenging. This article will attempt to bridge these gaps, by covering the evolution and current state of the tools at the disposal of sp-ICP-MS users.
Graphical Abstract
KW - Trend Article
KW - spICP-MS
KW - Data Tools
KW - scICP-MS
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610539
DO - https://doi.org/10.1007/s00216-024-05513-4
SP - 1
EP - 7
PB - Springer Science and Business Media LLC
AN - OPUS4-61053
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Breuninger, Esther S.
A1 - Tolu, Julie
A1 - Aemisegger, Franziska
A1 - Thurnherr, Iris
A1 - Bouchet, Sylvain
A1 - Mestrot, Adrien
A1 - Ossola, Rachele
A1 - McNeill, Kristopher
A1 - Tukhmetova, Dariya
A1 - Vogl, Jochen
A1 - Meermann, Björn
A1 - Sonke, Jeroen E.
A1 - Winkel, Lenny H. E.
T1 - Marine and terrestrial contributions to atmospheric deposition fluxes of methylated arsenic species
N2 - Arsenic, a toxic element from both anthropogenic and natural sources, reaches surface environments through atmospheric cycling and dry and wet deposition. Biomethylation volatilizes arsenic into the atmosphere and deposition cycles it back to the surface, affecting soil-plant systems. Chemical speciation of deposited arsenic is important for understanding further processing in soils and bioavailability. However, the range of atmospheric transport and source signature of arsenic species remain understudied. Here we report significant levels ofmethylated arsenic in precipitation, cloudwater and aerosols collected under free tropospheric conditions at Pic du Midi Observatory (France) indicating long-range transport, which is crucial for atmospheric budgets. Through chemical analyses andmoisture source diagnostics, we identify terrestrial and marine sources for distinct arsenic species. Estimated atmospheric deposition fluxes of methylated arsenic are similar to reported methylation rates in soils, highlighting atmospheric deposition as a significant, overlooked source of potentially bioavailable methylated arsenic
species impacting plant uptake in soils.
KW - Arsenic
KW - Speciation
KW - Fluxes
KW - Marine
KW - Terrestrial
KW - Sulfur isotopes
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615551
DO - https://doi.org/10.1038/s41467-024-53974-z
SN - 2041-1723
VL - 15
IS - 1
SP - 1
EP - 13
PB - Springer Science and Business Media LLC
AN - OPUS4-61555
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zweigle, J.
A1 - Schmidt, A.
A1 - Bugsel, B.
A1 - Vogel, Christian
A1 - Simon, Fabian
A1 - Zwiener, C.
T1 - Perfluoroalkyl acid precursor or weakly fluorinated organic compound? A proof of concept for oxidative fractionation of PFAS and organofluorines
N2 - Organofluorine mass balance approaches are increasingly applied to investigate the occurrence of per- and polyfluoroalkyl substances (PFAS) and other organofluorines in environmental samples more comprehensively. Usually, complex samples prevent the identification and quantification of every fluorine-containing molecule. Consequently, large unidentified fractions between fluorine sum parameters such as extractable organic fluorine (EOF) and the sum of quantified analytes are frequently reported. We propose using oxidative conversion to separate (unidentified) weakly fluorinated compounds (e.g., pesticides, pharmaceuticals) from PFAA-precursors (perfluoroalkyl chain lengths ≥ C6). We show with three organofluorine model substances (flufenamic acid, diflufenican, pantoprazole) that CF3-groups or aromatic fluorine can be quantitatively converted to inorganic fluoride and trifluoroacetic acid (TFA) by applying PhotoTOP oxidation (UV/TiO2). The principle of fluorine separation in mixtures is demonstrated by the oxidation of the three weakly fluorinated compounds together with the PFAA-precursor 6:2/6:2 fluorotelomer mercaptoalkyl phosphate diester (FTMAP). After oxidation, the products F− and TFA were separated from PFCAs ( C4) by SPE, and the fractions were analyzed individually. Closed mass balances both with and without the addition of organic matrix were achieved. Eventually, the fluorine balance was verified by total fluorine measurements with combustion ion chromatography (CIC). The proposed methods should be considered a proof of concept to potentially explain unidentified fractions of the EOF, especially if compounds with low fluorine content such as pesticides, pharmaceuticals, and their transformation products contribute largely to the EOF. Future studies are needed to show the applicability to the complexity of environmental samples.
Graphical Abstract
KW - Combustion Ion Chromatography
KW - Per- and Polyfluoroalkyl substances (PFAS)
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613429
DO - https://doi.org/10.1007/s00216-024-05590-5
SP - 1
EP - 10
PB - Springer Science and Business Media LLC
AN - OPUS4-61342
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - D'Agostino, Giancarlo
A1 - Oelze, Marcus
A1 - Vogl, Jochen
A1 - Ghestem, Jean-Philippe
A1 - Lafaurie, Nicolas
A1 - Klein, Ole
A1 - Pröfrock, Daniel
A1 - Di Luzio, Marco
A1 - Bergamaschi, Luigi
A1 - Jaćimović, Radojko
A1 - Oster, Caroline
A1 - Irrgeher, Johanna
A1 - Lancaster, Shaun T.
A1 - Walch, Anna
A1 - Röthke, Anita
A1 - Michaliszyn, Lena
A1 - Pramann, Axel
A1 - Rienitz, Olaf
A1 - Sara-Aho, Timo
A1 - Cankur, Oktay
A1 - Kutan, Derya
A1 - Noireaux, Johanna
T1 - Development and application of reference and routine analytical methods providing SI-traceable results for the determination of technology-critical elements in PCB from WEEE
N2 - The recovery and reprocessing of technology-critical elements (TCE) present in printed circuit boards (PCB) from electrical and electronic waste is essential both for recycling valuable materials subject to supply risk and for reducing the environmental impact. Although the quantitative knowledge of TCE amounts in endof- life PCB plays a key role, there are neither matrix certified reference materials nor harmonized analytical methods available to establish the traceability of the results to the International System of Units. To fill these gaps, we developed and applied five reference analytical methods based on ICP-MS standard addition calibrations and INAA k0- and relative calibrations suitable to certify reference materials. In addition, we developed and tested six analytical methods based on more commonly used ICP-MS external standard calibrations to provide industry with routine analysis methods. Twenty TCE (Ag, Au, Co, Cu, Dy, Ga, Gd, Ge, In, La, Li, Nd, Ni, Pd, Pr, Pt, Rh, Sm, Ta and Ti) were selected as target analytes and a batch of powdered PCB was used as measurement material. An overall mutual agreement was observed among data collected by reference methods at a few percent relative uncertainty levels. Moreover, all but one of the methods developed for routine analysis demonstrated their suitability in industrial applications by producing data within ± 20% of the values established with reference methods.
KW - Technology critical elements
KW - Electronic waste
KW - Printed circuit boards
KW - Traceability
KW - Uncertainty
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612416
DO - https://doi.org/10.1039/d4ja00235k
SN - 1364-5544
VL - 39
IS - 11
SP - 2809
EP - 2823
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-61241
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lancaster, Shaun T.
A1 - Sahlin, Eskil
A1 - Oelze, Marcus
A1 - Ostermann, Markus
A1 - Vogl, Jochen
A1 - Laperche, Valérie
A1 - Touze, Solène
A1 - Ghestem, Jean-Philippe
A1 - Dalencourt, Claire
A1 - Gendre, Régine
A1 - Stammeier, Jessica
A1 - Klein, Ole
A1 - Pröfrock, Daniel
A1 - Košarac, Gala
A1 - Jotanovic, Aida
A1 - Bergamaschi, Luigi
A1 - Di Luzio, Marco
A1 - D’Agostino, Giancarlo
A1 - Jaćimović, Radojko
A1 - Eberhard, Melissa
A1 - Feiner, Laura
A1 - Trimmel, Simone
A1 - Rachetti, Alessandra
A1 - Sara-Aho, Timo
A1 - Roethke, Anita
A1 - Michaliszyn, Lena
A1 - Pramann, Axel
A1 - Rienitz, Olaf
A1 - Irrgeher, Johanna
T1 - Evaluation of X-ray fluorescence for analysing critical elements in three electronic waste matrices: A comprehensive comparison of analytical techniques
N2 - As the drive towards recycling electronic waste increases, demand for rapid and reliable analytical methodology to analyse the metal content of the waste is increasing, e.g. to assess the value of the waste and to decide the correct recycling routes. Here, we comprehensively assess the suitability of different x-ray fluorescence spectroscopy (XRF)-based techniques as rapid analytical tools for the determination of critical raw materials, such as Al, Ti, Mn, Fe, Co, Ni, Cu, Zn, Nb, Pd and Au, in three electronic waste matrices: printed circuit boards (PCB), light emitting diodes (LED), and lithium (Li)-ion batteries. As validated reference methods and materials to establish metrological traceability are lacking, several laboratories measured test samples of each matrix using XRF as well as other independent complementary techniques (instrumental neutron activation analysis (INAA), inductively coupled plasma mass spectrometry (ICP-MS) and ICP optical emission spectrometry (OES)) as an inter-laboratory comparison (ILC). Results highlighted key aspects of sample preparation, limits of detection, and spectral interferences that affect the reliability of XRF, while additionally highlighting that XRF can provide more reliable data for certain elements compared to digestion-based approaches followed by ICP-MS analysis (e.g. group 4 and 5 metals). A clear distinction was observed in data processing methodologies for wavelength
dispersive XRF, highlighting that considering the metals present as elements (rather than oxides) induces overestimations of the mass fractions when compared to other techniques. Eventually, the effect of sample particle size was studied and indicated that smaller particle size (<200 μm) is essential for reliable determinations.
KW - XRF
KW - WEEE
KW - PCB
KW - Battery
KW - LED
KW - Recycling
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614060
DO - https://doi.org/10.1016/j.wasman.2024.10.015
VL - 190
SP - 496
EP - 505
PB - Elsevier B.V.
AN - OPUS4-61406
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gregório, Bruno J.R.
A1 - Ramos, Inês I.
A1 - Marques, Sara S.
A1 - Barreiros, Luísa
A1 - Magalhães, Luís M.
A1 - Schneider, Rudolf
A1 - Segundo, Marcela A.
T1 - Microcarrier-based fluorescent yeast estrogen screen assay for fast determination of endocrine disrupting compounds
N2 - The presence of endocrine-disrupting compounds (EDCs) in water poses a significant threat to human and animal health, as recognized by regulatory agencies throughout the world. The Yeast Estrogen Screen (YES) assay is an excellent method to evaluate the presence of these compounds in water due to its simplicity and capacity to assess the bioaccessible forms/fractions of these compounds. In the presence of a compound with estrogenic activity, Saccharomyces cerevisiae cells, containing a lacZ reporter gene encoding the enzyme β-galactosidase, are induced, the enzyme is synthesised, and released to the extracellular medium. In this work, a YES-based approach encompassing the use of a lacZ reporter gene modified strain of S. cerevisiae, microcarriers as solid support, and a fluorescent substrate, fluorescein di-β-D-galactopyranoside, is proposed, allowing for the assessment of EDCs’ presence after only 2 h of incubation. The proposed method provided an EC50 of 0.17 ± 0.03 nM and an LLOQ of 0.03 nM, expressed as 17β-estradiol. The assessment of different EDCs provided EC50 values between 0.16 and 1.2 × 103 nM. After application to wastewaters, similar results were obtained for EDCs screening, much faster, compared to the conventional 45 h spectrophotometric procedure using a commercial kit, showing potential for onsite high-throughput screening of environmental contamination.
KW - Biosensoren
KW - YES assay
KW - Endokrine Disruptoren
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602315
DO - https://doi.org/10.1016/j.talanta.2024.125665
VL - 271
SP - 1
EP - 7
PB - Elsevier B.V.
CY - Amsterdam
AN - OPUS4-60231
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -