TY - RPRT
A1 - Thünemann, Andreas
A1 - Emmerling, Franziska
A1 - Hodoroaba, Vasile-Dan
T1 - Review of existing calibration or reference
N2 - We report on calibration standards of nanoparticles meeting the definition of a nanomaterial given by the European Commission (EU 2011) which are relevant for the characterisation methods applied in the NanoDefine project. We found that the Impact of nanoparticles is outstanding in the scientific literature. A number of 270.000 paper titles on nanoparticles are listed in the Web of Science data base. But surprisingly, the availability of suitable certified standard reference materials is scarce. Only a few sources were found. For example, BAM provides the database Nanoscaled Reference Materials at http://www.nano-refmat.bam.de/en/ in cooperation with the ISO/TC 229 Nanotechnologies. In addition, two publications from 2013 on nanoscale reference materials are available. Candidates of nano-(certified) reference materials from other ongoing or just finished FP6 and FP7 nano-metrology projects have been extracted from the Compendium of Projects in the European NanoSafety Cluster (Compendium NSC, 2013). Recommendations for selection of representative test materials and calibration standards for NanoDefine internal tasks, respectively, are also given.
KW - Nanomaterial
KW - Reference materials
KW - Certified reference materials
PY - 2014
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389836
UR - http://www.nanodefine.eu/index.php/downloads/nanodefine-technical-reports
SP - 1
EP - 18
CY - Wageningen, The Netherlands
AN - OPUS4-38983
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Haferkamp, Sebastian
A1 - Fischer, Franziska
A1 - Kraus, Werner
A1 - Emmerling, Franziska
T1 - Mechanochemical Knoevenagel condensation investigated in situ
N2 - The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction.
KW - Mechanochemistry
KW - Ball milling
KW - C–C coupling
KW - In situ
KW - Knoevenagel condensation
PY - 2017
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-425388
DO - https://doi.org/10.3762/bjoc.13.197
VL - 13
SP - 2010
EP - 2014
PB - Beilstein-Institut
AN - OPUS4-42538
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Haugen, Øyvind P.
A1 - Polanco-Garriz, Itziar
A1 - Alcolea-Rodriguez, Victor
A1 - Portela, Raquel
A1 - Bæra, Rita
A1 - Sadeghiankaffash, Hamed
A1 - Hildebrandt, Jana
A1 - Ciornii, Dmitri
A1 - Altmann, Korinna
A1 - Barbero, Francesco
A1 - Fenoglio, Ivana
A1 - Reinosa, Julián J.
A1 - Fernández, José F.
A1 - Katsumiti, Alberto
A1 - Camassa, Laura M.A.
A1 - Wallin, Håkan
A1 - Zienolddiny-Narui, Shan
A1 - Afanou, Anani K.
T1 - Activation of Toll-like receptor 2 reveals microbial contamination beyond endotoxins on micro- and nanoplastics
N2 - Current literature on health hazards associated with micro- and nanoplastics (MNPs) is largely influenced by studies that insufficiently account for potential microbial contamination of their test materials. This may lead to misinterpretation of outcomes, as the test materials may be incorrectly considered pristine MNPs. The present study screened eight MNP test materials for microbial contaminants using Toll-like receptor (TLR) reporter cells for TLR2 and TLR4 and the commonly used Limulus amebocyte lysate (LAL) assay. Our results show that MNPs testing negative for endotoxins, based on the absence of TLR4 activation and negative LAL results, may still contain microbial ligands that selectively activate TLR2. Moreover, five of the eight MNP test materials contained microbial ligands capable of activating TLR2 and/or TLR4. Compared to the LAL assay, TLR4-based screening effectively detected endotoxin contamination. Overall, we found that the TLR reporter cell assay provides broader coverage than the LAL assay in detecting microbial ligands, which appear to be highly prevalent in MNP test materials.
KW - Nanoplastics
KW - Microplastics
KW - Microbial contamination
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653286
DO - https://doi.org/10.1016/j.tiv.2025.106190
SN - 0887-2333
VL - 112
SP - 1
EP - 8
PB - Elsevier Ltd.
AN - OPUS4-65328
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Putzu, Mara
A1 - Wiesner, Yosri
A1 - Weimann, Christiane
A1 - Hodoroaba, Vasile-Dan
A1 - Muniategui Lorenzo, Soledad
A1 - Fernández-Gonzáles, Verónica
A1 - Booth, Andy M.
A1 - Igartua, Amaia
A1 - Benismail, Nizar
A1 - Coïc, Laureen
A1 - Chivas-Joly, Carine
A1 - Fenoglio, Ivana
A1 - Rossi, Andrea Mario
A1 - Giovannozzi, Andrea Mario
A1 - Altmann, Korinna
T1 - Optimization of tablet processing as a reference material for microplastic detection methods
N2 - Reference materials (RMs) are essential and highly demanded tools for the development and validation of methods for microplastic (MP) quantification in complex matrices, to ensure comparable and harmonized approaches aligned with EU commission criteria for monitoring MPs (e.g., Drinking Water Directive and Urban Wastewater Treatment Directive). This study investigates different approaches for optimizing the production of polypropylene (PP) RMs in the form of water-soluble tablets, which were carefully evaluated for their homogeneity and stability according to ISO Guide 30, ISO 33401, and ISO 33405. PP particles (1–100 μm) were produced by cryomilling and embedded in a lactose/PEG matrix, then pressed into tablets (18 µg theoretical PP mass). The production process was optimized by varying (i) the size distribution of the matrix components and (ii) the mixer instrument. The materials obtained were characterized by thermogravimetric analysis to assess the homogeneity distribution of MPs with respect to PP mass in the individual tablets and their stability over a 4-month period. The most promising approach, with a homogenous mass of 19 μg (standard deviation of 4 μg), relative standard deviation of 19%, was further investigated for homogeneity by comparison with thermo-analytical mass determination methods, such as TED-GC/MS (thermal extraction desorption-gas chromatography/mass spectrometry) and Py-GC/MS (pyrolysis-gas chromatography-mass spectrometry), and for number-based characterization using micro-Raman spectroscopy. Material characterization was also examined using laser diffraction, scanning electron microscopy, and ATR-FTIR. Based on the results, the optimized processing protocol yields a PP RM suitable for quality control and method performance studies supporting standardization.
KW - Microplastics
KW - TED-GC/MS
KW - Reference materials
KW - Polypropylene
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653290
DO - https://doi.org/10.1007/s00216-025-06271-7
SN - 1618-2642
SP - 1
EP - 14
PB - Springer Science and Business Media LLC
AN - OPUS4-65329
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wiesner, Yosri
A1 - Eisentraut, Paul
A1 - Altmann, Korinna
T1 - One Year Observation of Microplastic Concentrations in the River Rhine
N2 - In recent years, the quantification of microplastics (MP) in aquatic environments has gained increasing attention, particularly regarding their environmental distribution and potential exposure levels. Environmentally relevant exposure data are still essential for a realistic risk assessment of the harmful health potential of microplastics in freshwater systems. This study addresses a large data set of MP concentrations analyzed and processed under statistical aspects and provides mass concentrations as well as associated size fractions of the detected MP. Over a 12 month period, samples were collected at three locations and analyzed across three particle size fractions (100−500 μm, 50−100 μm, and 10−50 μm) using thermalextraction desorption-gas chromatography/mass spectrometry (TED-GC/MS). The most prevalent polymers identified were polyethylene (PE), polypropylene (PP), polystyrene (PS), styrene−butadiene rubber (SBR), and natural rubber (NR). Statistical analyses, including principal component and cluster analysis, revealed size-dependent patterns,minor seasonal variation and spatial variations. These findings are particularly significant for ecotoxicological research and regulatory development, especially regarding tire abrasion a rarely quantified but potentially harmful MP source. The study contributes aluable data for future environmental monitoring and supports EU directives on wastewater and drinking water quality
KW - TED-GC/MS
KW - Microplastics
KW - Environment
KW - Monitoring
KW - Reference data
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654669
DO - https://doi.org/10.1021/acsestwater.5c00530
SN - 2690-0637
SP - 1
EP - 10
PB - American Chemical Society (ACS)
AN - OPUS4-65466
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hemingway, Jack M.
A1 - Quayle, Heather M.
A1 - Byrne, Cian
A1 - Pulham, Colin R.
A1 - Mondal, Subrata
A1 - Michalchuk, Adam
A1 - Morrison, Carole A.
T1 - Predicting impact sensitivities for an extended set of energetic materials via the vibrational up-pumping model: Molecular-based structure–property relationships identified
N2 - We have applied the vibrational up-pumping model to predict the mechanically-induced impact sensitivities of 33 molecular energetic crystals. Overall, the current model successfully identifies and ranks the compounds that are most sensitive to mechanical initiation, but offers poorer differentiation between compounds with lower sensitivity. Further developments to include the effects of trigger bond activation led to significant improvements in predictive capability. We show that this structure–property model highlights the importance of molecular flexibility in predicting impact sensitivity, and furthermore, we show that the Kier molecular flexibility index, which can be obtained from a SMILES string, offers a simple molecular-based descriptor that goes some way towards predicting the sensitivity of energetic materials.
KW - Vibrational
KW - Pyrazoles
KW - Comprising
KW - Electronic
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632651
DO - https://doi.org/10.1039/d5cp00852b
SN - 1463-9076
VL - 27
IS - 22
SP - 11640
EP - 11648
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-63265
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ghiringhelli, Luca M.
A1 - Baldauf, Carsten
A1 - Bereau, Tristan
A1 - Brockhauser, Sandor
A1 - Carbogno, Christian
A1 - Chamanara, Javad
A1 - Cozzini, Stefano
A1 - Curtarolo, Stefano
A1 - Draxl, Claudia
A1 - Dwaraknath, Shyam
A1 - Fekete, Ádám
A1 - Kermode, James
A1 - Koch, Christoph T.
A1 - Kühbach, Markus
A1 - Ladines, Alvin Noe
A1 - Lambrix, Patrick
A1 - Himmer, Maja-Olivia
A1 - Levchenko, Sergey V.
A1 - Oliveira, Micael
A1 - Michalchuk, Adam
A1 - Miller, Ronald E.
A1 - Onat, Berk
A1 - Pavone, Pasquale
A1 - Pizzi, Giovanni
A1 - Regler, Benjamin
A1 - Rignanese, Gian-Marco
A1 - Schaarschmidt, Jörg
A1 - Scheidgen, Markus
A1 - Schneidewind, Astrid
A1 - Sheveleva, Tatyana
A1 - Su, Chuanxun
A1 - Usvyat, Denis
A1 - Valsson, Omar
A1 - Wöll, Christof
A1 - Scheffler, Matthias
T1 - Shared metadata for data-centric materials science
N2 - The expansive production of data in materials science, their widespread sharing and repurposing requires educated support and stewardship. In order to ensure that this need helps rather than hinders scientific work, the implementation of the FAIR-data principles (Findable, Accessible, Interoperable, and Reusable) must not be too narrow. Besides, the wider materials-science community ought to agree on the strategies to tackle the challenges that are specific to its data, both from computations and experiments. In this paper, we present the result of the discussions held at the workshop on “Shared Metadata and Data Formats for Big-Data Driven Materials Science”. We start from an operative definition of metadata, and the features that a FAIR-compliant metadata schema should have. We will mainly focus on computational materials-science data and propose a constructive approach for the FAIRification of the (meta)data related to ground-state and excited-states calculations, potential-energy sampling, and generalized workflows. Finally, challenges with the FAIRification of experimental (meta)data and materials-science ontologies are presented together with an outlook of how to meet them.
KW - Library and Information Sciences
KW - Statistics, Probability and Uncertainty
KW - Computer Science Applications
KW - Education
KW - Information Systems
KW - Statistics and Probability
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584846
DO - https://doi.org/10.1038/s41597-023-02501-8
VL - 10
IS - 1
SP - 1
EP - 18
PB - Springer Science and Business Media LLC
AN - OPUS4-58484
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Michalchuk, Adam
T1 - On the physical processes of mechanochemically induced transformations in molecular solids
N2 - Initiating or sustaining physical and chemical transformations with mechanical force – mechanochemistry – provides an opportunity for more sustainable chemical processes, and access to new chemical reactivity.
KW - Molecular solids
KW - Transformation
KW - Destabilisation
KW - Instabilities
KW - Common phenomenon
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621755
DO - https://doi.org/10.1039/d4cc04062g
IS - 99
SP - 1
EP - 12
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-62175
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Driscoll, Laura L.
A1 - Driscoll, Elizabeth H.
A1 - Dong, Bo
A1 - Sayed, Farheen N.
A1 - Wilson, Jacob N.
A1 - O’Keefe, Christopher A.
A1 - Gardner, Dominic J.
A1 - Grey, Clare P.
A1 - Allan, Phoebe K.
A1 - Michalchuk, Adam
A1 - Slater, Peter R.
T1 - Under pressure: offering fundamental insight into structural changes on ball milling battery materials
N2 - Synthesis of Li ion battery materials via ball milling has been a huge area of growth, leading to new high-capacity electrode materials, such as a number of promising disordered rocksalt (DRS) phases. In prior work, it was generally assumed that the synthesis was facilitated simply by local heating effects during the milling process. In this work, we show that ball milling Li2MoO4 leads to a phase transformation to the high pressure spinel polymorph and we report electrochemical data for this phase. This observation of the formation of a high pressure polymorph shows that local heating effects alone cannot explain the phase transformation observed (phenakite to spinel) and so indicates the importance of other effects. In particular, we propose that when the milling balls collide with the material, the resulting shockwaves exert a localised pressure effect, in addition to local heating. To provide further support for this, we additionally report ball milling results for a number of case studies (Li2MnO3, Li2SnO3, Nb2O5) which reinforces the conclusion that local heating alone cannot explain the phase transformations observed. The work presented thus provides greater fundamental understanding of milling as a synthetic pathway and suggests potential strategies to prepare such samples without milling (e.g., doping to create internal chemical pressure). In addition, we suggest that further research is needed into the effect of the use of milling as a route to smaller particles, since we believe that such milling may also be affecting the surface structure of the particles through the influence of the shockwaves generated.
KW - Pollution
KW - Nuclear Energy and Engineering
KW - Sustainability and the Environment
KW - Environmental Chemistry
KW - Renewable Energy
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590086
DO - https://doi.org/10.1039/d3ee00249g
VL - 16
IS - 11
SP - 5196
EP - 5209
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59008
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dudziak, Mateusz
A1 - Riechers, Birte
A1 - Maaß, Robert
A1 - Michalchuk, Adam
A1 - Schönhals, Andreas
A1 - Szymoniak, Paulina
T1 - Beyond conventional calorimetry: Unlocking thermal characterization with fast scanning techniques
N2 - Fast scanning calorimetry (FSC) has emerged as a transformative technique in thermal analysis, enabling the investigation of rapid and kinetically driven thermal transitions that are inaccessible to conventional differential scanning calorimetry. This review highlights the capabilities enabled by FSC for studying a wide range of materials under extreme thermal conditions, including polymers, pharmaceuticals, metallic glasses, nanocomposites, and hydrogels. By employing ultrafast heating and cooling rates, FSC allows for the suppression of crystallization, resolution of weak transitions, and analysis of thermally labile or size-limited samples. The technique is particularly valuable for probing glass transitions, relaxation phenomena, and phase behavior in systems with complex morphologies or confined geometries. Case studies demonstrate the use of FSC in characterizing vitrification, physical aging, and interfacial dynamics, as well as its application in emerging fields such as additive manufacturing, supramolecular systems, and neuromorphic materials. Together, these examples underscore the role that FSC plays in advancing the understanding of structure-property relationships across diverse material classes.
KW - Flash DSC
KW - Calorimetry
KW - Glass transition
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647405
DO - https://doi.org/10.1016/j.tca.2025.180177
VL - 754
SP - 1
EP - 14
PB - Elsevier B.V.
AN - OPUS4-64740
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Linberg, Kevin
A1 - Szymoniak, Paulina
A1 - Schönhals, Andreas
A1 - Emmerling, Franziska
A1 - Michalchuk, Adam
T1 - The Origin of Delayed Polymorphism in Molecular Crystals Under Mechanochemical Conditions
N2 - We show that mechanochemically driven polymorphic transformations can require extremely long induction periods, which can be tuned from hours to days by changing ball milling energy. The robust design and interpretation of ball milling experiments must account for this unexpected kinetics that arises from energetic phenomena unique to the solid state. Detailed thermal analysis, combined with DFT simulations, indicates that these marked induction periods are associated with processes of mechanical activation. Correspondingly, we show that the pre‐activation of reagents can also lead to marked changes in the length of induction periods. Our findings demonstrate a new dimension for exerting control over polymorphic transformations in organic crystals. We expect mechanical activation to have a much broader implication across organic solid‐state mechanochemistry.
KW - General Chemistry
KW - Catalysis
KW - Organic Chemistry
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589219
DO - https://doi.org/10.1002/chem.202302150
SN - 0947-6539
SP - e202302150
PB - Wiley
AN - OPUS4-58921
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gugin, Nikita
A1 - Yusenko, Kirill
A1 - King, Andrew
A1 - Meyer, Klas
A1 - Al-Sabbagh, Dominik
A1 - Villajos Collado, José Antonio
A1 - Emmerling, Franziska
T1 - Lighting up industrial mechanochemistry: Real-time in situ monitoring of reactive extrusion using energy-dispersive X-ray diffraction
N2 - Mechanochemistry is an environmentally friendly synthetic approach that enables the sustainable production of a wide range of chemicals while reducing or eliminating the need for solvents. Reactive extrusion aims to move mechanochemistry from its conventional gram-scale batch reactions, typically performed in laboratory ball mills, to a continuous, large-scale process. Meeting this challenge requires in situ monitoring techniques to gain insights into reactive extrusion and its underlying processes. While the effectiveness of in situ Raman spectroscopy in providing molecular-level information has been demonstrated, our study uses energy-dispersive X-ray diffraction to monitor reactive extrusion in real time at the crystalline level. Our results provide previously unavailable control over the reactive extrusion process, promoting its perception as an industrially feasible green alternative to traditional solvent-based syntheses.
KW - Mechanochemistry
KW - Reactive extrusion
KW - Green chemistry
KW - In situ studies
KW - Time-resolved in situ
KW - TRIS
KW - Synchrotron radiation
KW - Scalable synthesis
KW - Solid-state reactions
KW - Reaction mechanisms
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613969
DO - https://doi.org/10.1016/j.chempr.2024.07.033
VL - 10
IS - 11
SP - 1
EP - 16
PB - Elsevier B.V.
AN - OPUS4-61396
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wimmer, L
A1 - Hoang, M V N
A1 - Schwarzinger, J
A1 - Jovanovic, V
A1 - Adelkovic, B
A1 - Velickovic, T C
A1 - Meisel, T C
A1 - Waniek, T
A1 - Weimann, Christiane
A1 - Altmann, Korinna
A1 - Dailey, L A
T1 - A quality-by-design inspired approach to develop PET and PP nanoplastic test materials for use in in vitro and in vivo biological assays
N2 - Micro- and nanoplastics have become environmental pollutants of concern, receiving increased attention from consumers, scientists, and policymakers. The lack of knowledge about possible impacts on wildlife and human health requires further research, for which well-characterized testmaterials are needed. A quality-bydesign (QbD) driven approachwas used to produce sterile, endotoxinmonitored nanoplastics of polyethylene terephthalate (PET) and polypropylene (PP) with a size fraction of >90% below 1 μm and high yield of >90%. Glycerol was used as a versatile and biocompatible liquid storage medium which requires no further exogenous dispersing agent andmaintained colloidal stability, sterility (0 CFU mL−1), and low endotoxin levels (<0.1 EU mL−1) for more than one year of storage at room temperature. Further, the glycerol vehicle showed no biological effect on the tested human bronchial cell line Calu-3 up to 0.8% (w/v). Given the concentration of 40 mg g−1 nanoplastics in the glycerol stock, this corresponds to a nanoplastic concentration of 320 μg mL−1. The surfactant-free nanoplastics are dispersible in bio-relevant media from the glycerol stock without changing size characteristics and are suitable for in vitro and in vivo research.
KW - Microplastics
KW - Reference materials
KW - Nanoplastics
KW - Polymer 3R
KW - Glycerol
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629934
DO - https://doi.org/10.1039/D4EN01186D
SN - 2051-8161
VL - 12
IS - 5
SP - 2667
EP - 2686
PB - Royal Society of Chemistry
CY - Cambridge
AN - OPUS4-62993
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 - Rodríguez-Sánchez, Noelia
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Prinz, Carsten
A1 - Prieto-Laria, P.
A1 - Ruiz-Salvador, A.R.
A1 - Ballesteros, M.
T1 - Engineering a multivariate cobalt metal–organic framework for high photocatalytic activity: the impact of mixed ligands and metal incorporation in a visible light-driven heterogeneous photo-Fenton reaction for water treatment
N2 - Metal–organic frameworks (MOFs) have attracted increasing attention for the removal of organic pollutants in wastewater via photocatalysis. Here, we design a multivariate modification of ZIF-9 to tune its electronic properties for use in visible light photocatalysis. A controllable synthesis of ZIF-9 and its multivariate forms with the incorporation of copper and the 2-imidazolecarboxaldehyde (ica) ligand was carried out. The materials are tested for the removal of the model dye methylene blue (MB) by a heterogeneous photo-Fenton-like reaction at neutral pH and room temperature. Cu-ZIF-9-ica (UPO-3) shows high photocatalytic activity under both visible and ultraviolet A (UVA) light, achieving 94% MB degradation in 45 min, compared to 65% MB degradation in 120 min using bare ZIF-9. The study revealed a first-order rate constant of 0.0475 min−1 for Cu-ZIF-9-ica compared to 0.0088 min−1 for ZIF-9 under visible light. The improvement of the catalyst was clearly attributed to the co-incorporation of Cu and the ica ligand in the MOF, which reduces the band gap, in agreement with DFT calculations. Reproducibility and recyclability tests proved that Cu-ZIF-9-ica can be used for at least 3 cycles without a significant loss of efficiency, making it a promising material for the study and application of wastewater treatment.
KW - Metal-Organic Framework (MOF)
KW - Heterogeneous photo-Fenton
KW - ZIF-9
KW - Methylene Blue
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630797
DO - https://doi.org/10.1039/d4na00954a
SN - 2516-0230
VL - 7
IS - 8
SP - 2255
EP - 2265
PB - Royal Society of Chemistry
AN - OPUS4-63079
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Visileanu, Emilia
A1 - Catalin Grosu, Marian
A1 - Tiberiu Miclea, Paul
A1 - Altmann, Korinna
A1 - Brossell, Dirk
T1 - Methods for the collection and characterization of airborne particles in the textile industry
N2 - Airborne particulate matter is one of the main air pollutants. Their impact on mortality, and the occurrence of pulmonary and cardiovascular complications, have been the subject of numerous studies. Airborne particles are complex mixtures of organic and inorganic substances from different sources of particle emissions. Particulate Matter (PM) particles are classified according to their aerodynamic diameter expressed in µm and can vary from coarse (PM 10) to fine (less than PM 2.5). These diameter considerations are fundamental because they condition the penetration of particles into the bronchopulmonary system and the body. In recent years, there has been an interest in so-called “ultra-fine” particles, with a diameter of 0.1 µm (or 100 nm), or PM 0.1. They are nanoparticles and their impact on human health is not yet clear.With more than 1.5 million employees, textiles and clothing is a diverse sector that plays an important role in the European manufacturing industry, producing a turnover of €162 billion.An important component of the solid particles that generate air pollution in the textile industry is microplastics (MP) and nano plastics (NP), which also include microfibers (<5mm) and nanofibers (<100 nm), respectively. The particles released into the air during fiber and yarn processing range from 1 µg/m3 to 50 µg/m3.The paper presents the results of the determination of indoor and outdoor air concentration levels in textile companies, to identify the areas with the highest concentration level, by using an online recording system such as the Laser Aerosol Spectrometer MINI LAS model 11-E. The total concentration level TSP (µg/m3), the fractions PM 10(µg/m3), PM 2.5(µg/m3), PM1(µg/m3), as well as the total number of particles TC (1/l), were shown. It was noted that TSP is approximately at the same level both indoors and outdoors, but the fractions of PM10, PM2.5, and PM1 have much higher values indoors than outdoors with possible consequences on workers' health.The next step was the collection of fibers, namely micro and nano plastic particles from the vicinity of the workplaces of polyester, polyamide, and polypropylene fibers processing units in the textile industry in Romania, to obtain a sufficient quantity for laboratory analysis to determine the size and shape of the particles as well as their chemical composition. Two types of pumps were used, differentiated by their operating parameters: TECORA SKYPOST with airflow of 38 l/min and GILAIRPLUS with airflow 2l/min. Filters made of different materials with different diameters and pore sizes were used, namely: quartz filters (ø 47 mm, and ø 37 mm) on a TECORA SKYPOST type pump, polycarbonate nucleopore coated with a gold membrane (ø 25 mm) and silica filter (ø 9 mm) on GILAIRPLUS type pump.Using descriptive statistics, the calculation of correlation coefficients highlighted a strong correlation between the variables: "Collected mass/ Air concentration" and "Collected mass/ Air volume" for all diameters of the filters.The highest collected particle volume, determined by weighing the filters before and after collection, was obtained with the quartz filters (ø 47 mm) at an airflow of 38 l/min. The particles collected (polyester, polyamide, polypropylene) in the first stage were analyzed by SEM and thermogravimetric and it was found that the quartz filters absorbed the particles inside, with very few remaining on the surface. Thus no known methods can be used to perform analysis for particles collected on quartz filters. The number of particles on the filters was insufficient for analysis either because of the collection parameters used or because of the loss of particles during transport. As a result, in the next step, the use of 9 mm Si filters using the GILAIRPLUS pump at an airflow rate of 2l/min was chosen.To improve the transport conditions and avoid the loss of the particles and keep them on the surface of the filters, two methods were applied:- after weighing the filters were reintroduced into the collection pump holder;- a filtration system for airborne micro-nano plastics was designed and manufactured to selectively collect and transport PM10 and PM1 particles collected on SI filters.In both cases, SEM, Raman mapping, and GS-MS microscopy were used for analysis.Several times more PM10 than PM1 (74.5µg compared to 12.5 µg) was found. In all cases, both particles and fibers showed the same Raman fingerprint.The GS-MS analyses showed some contamination of the workspaces with particles other than the processed fibers. The presence of non-notifiable substances was also observed.The most viable filters are Si filters with a pore size of 10 microns to 1 micron and the use of the selected collection and transport filter system. In the following a filter system will be applied for collection on Au membrane-coated polycarbonate filters.
T2 - 5th International Conference on Human Systems Engineering and Design: Future Trends and Applications (IHSED 2023)
KW - Microplastics
KW - Textiles
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624442
DO - https://doi.org/10.54941/ahfe1004132
VL - 112
SP - 212
EP - 223
PB - AHFE International
AN - OPUS4-62444
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Emmerling, Franziska
ED - Rogge, Andreas
ED - Meng, Birgit
T1 - Exploring new materials for Green Intelligent Building - How can our BAMline help?
N2 - In the scope of exploring and characterizing new materials related to Green Intelligent Building (GIB), we will provide an overview of the X-ray spectroscopy and diffraction analytical methods available at the BAMline /1/. and Myspot beamlines. These are two universal beamlines at the Berlin Synchrotron BESSY-II, where BAM has access and supervision role. Overarching electronic and structural properties at different time and length scales, such measurements enable a real-time characterization of materials properties. We will show-case in situ and ex situ deterioration and hydration studies on cement-based constructure materials.
T2 - 11. Jahrestagung des DAfStb mit 63. Forschungskolloquium der BAM Green Intelligent Building
CY - Berlin, Germany
DA - 16.10.2024
KW - BAMline
KW - Scope of exploring
KW - Green intelligent building
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612882
SN - 978-3-9818564-7-7
SP - 30
EP - 36
PB - Bundesanstalt für Materialforschung und -prüfung (BAM)
CY - Berlin
AN - OPUS4-61288
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kader, A.
A1 - Snellings, J.
A1 - Adams, L. C.
A1 - Gottheil, P.
A1 - Mangarova, D. B.
A1 - Heyl, J. L.
A1 - Kaufmann, Jan Ole
A1 - Moeckel, J.
A1 - Brangsch, J.
A1 - Auer, T. A.
A1 - Collettini, F.
A1 - Sauer, F.
A1 - Hamm, B.
A1 - Käs, J.
A1 - Sack, I.
A1 - Makowski, M. R.
A1 - Braun, J.
T1 - Sensitivity of magnetic resonance elastography to extracellular matrix and cell motility in human prostate cancer cell line-derived xenograft models
N2 - Prostate cancer (PCa) is a significant health problem in the male population of the Western world. Magnetic resonance elastography (MRE), an emerging medical imaging technique sensitive to mechanical properties of biological tissues, detects PCa based on abnormally high stiffness and viscosity values. Yet, the origin of these changes in tissue properties and how they correlate with histopathological markers and tumor aggressiveness are largely unknown, hindering the use of tumor biomechanical properties for establishing a noninvasive PCa staging system.
To infer the contributions of extracellular matrix (ECM) components and cell motility, we investigated fresh tissue specimens from two PCa xenograft mouse models, PC3 and LNCaP, using magnetic resonance elastography (MRE), diffusion-weighted imaging (DWI), quantitative histology, and nuclear shape analysis. Increased tumor stiffness and impaired water diffusion were observed to be associated with collagen and elastin accumulation and decreased cell motility. Overall, LNCaP, while more representative of clinical PCa than PC3, accumulated fewer ECM components, induced less restriction of water diffusion, and exhibited increased cell motility, resulting in overall softer and less viscous properties. Taken together, our results suggest that prostate tumor stiffness increases with ECM accumulation and cell adhesion - characteristics that influence critical biological processes of cancer development.
MRE paired with DWI provides a powerful set of imaging markers that can potentially predict prostate tumor development from benign masses to aggressive malignancies in patients. Statement of significance: Xenograft models of human prostate tumor cell lines, allowing correlation of microstructure-sensitive biophysical imaging parameters with quantitative histological methods, can be investigated to identify hallmarks of cancer.
KW - Magnetic resonance elastography
KW - Quantitative histology
KW - Prostate cancer
KW - Stiffness
KW - Fluidity
KW - Apparent diffusion coefficient
KW - Collagen
KW - Elastin
KW - Nuclear shape
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618361
DO - https://doi.org/10.1016/j.bioadv.2024.213884
SN - 2772-9508
VL - 161
SP - 1
EP - 12
PB - Elsevier
CY - Amsterdam
AN - OPUS4-61836
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mangarova, Dilyana Branimirova
A1 - Reimann, Carolin
A1 - Kaufmann, Jan Ole
A1 - Möckel, Jana
A1 - Kader, Avan
A1 - Adams, Lisa Christine
A1 - Ludwig, Antje
A1 - Onthank, David
A1 - Robinson, Simon
A1 - Karst, Uwe
A1 - Helmer, Rebecca
A1 - Botnar, Rene
A1 - Hamm, Bernd
A1 - Makowski, Marcus Richard
A1 - Brangsch, Julia
T1 - Elastin-specific MR probe for visualization and evaluation of an interleukin-1β targeted therapy for atherosclerosis
N2 - Atherosclerosis is a chronic inflammatory condition of the arteries and represents the primary cause of various cardiovascular diseases. Despite ongoing progress, finding effective anti-inflammatory therapeutic strategies for atherosclerosis remains a challenge. Here, we assessed the potential of molecular magnetic resonance imaging (MRI) to visualize the effects of 01BSUR, an anti-interleukin-1β monoclonal antibody, for treating atherosclerosis in a murine model. Male apolipoprotein E-deficient mice were divided into a therapy group (01BSUR, 2 × 0.3 mg/kg subcutaneously, n = 10) and control group (no treatment, n = 10) and received a high-fat diet for eight weeks. The plaque burden was assessed using an elastin-targeted gadolinium-based contrast probe (0.2 mmol/kg intravenously) on a 3 T MRI scanner. T1-weighted imaging showed a significantly lower contrast-to-noise (CNR) ratio in the 01BSUR group (pre: 3.93042664; post: 8.4007067) compared to the control group (pre: 3.70679168; post: 13.2982156) following administration of the elastin-specific MRI probe (p < 0.05). Histological examinations demonstrated a significant reduction in plaque size (p < 0.05) and a significant decrease in plaque elastin content (p < 0.05) in the treatment group compared to control animals. This study demonstrated that 01BSUR hinders the progression of atherosclerosis in a mouse model. Using an elastin-targeted MRI probe, we could quantify these therapeutic effects in MRI.
N2 - Atherosklerose ist eine chronische entzündliche Erkrankung der Arterien und die Hauptursache für verschiedene Herz-Kreislauf-Erkrankungen. Trotz kontinuierlicher Fortschritte ist es nach wie vor schwierig, wirksame entzündungshemmende Therapiestrategien für Atherosklerose zu finden. In dieser Studie haben wir das Potenzial der molekularen Magnetresonanztomographie (MRT) zur Visualisierung der Wirkung von 01BSUR, einem monoklonalen Anti-Interleukin-1β-Antikörper, zur Behandlung von Atherosklerose in einem Mausmodell untersucht. Männliche Apolipoprotein-E-defiziente Mäuse wurden in eine Therapiegruppe (01BSUR, 2 × 0,3 mg/kg subkutan, n = 10) und eine Kontrollgruppe (keine Behandlung, n = 10) aufgeteilt und erhielten acht Wochen lang eine fettreiche Diät. Die Plaquebelastung wurde mit einer auf Elastin ausgerichteten Kontrastmittelsonde auf Gadoliniumbasis (0,2 mmol/kg intravenös) auf einem 3-T-MRT-Scanner untersucht. Die T1-gewichtete Bildgebung zeigte ein signifikant niedrigeres Kontrast-Rausch-Verhältnis (CNR) in der 01BSUR-Gruppe (vorher: 3,93042664; nachher: 8,4007067) im Vergleich zur Kontrollgruppe (vorher: 3,70679168; nachher: 13,2982156) nach Verabreichung der Elastin-spezifischen MRT-Sonde (p < 0,05). Histologische Untersuchungen zeigten eine signifikante Verringerung der Plaque-Größe (p < 0,05) und eine signifikante Abnahme des Plaque-Elastin-Gehalts (p < 0,05) in der Behandlungsgruppe im Vergleich zu den Kontrolltieren. Diese Studie zeigte, dass 01BSUR das Fortschreiten der Atherosklerose in einem Mausmodell hemmt. Mit einer auf Elastin ausgerichteten MRT-Sonde konnten wir diese therapeutischen Effekte in der MRT quantifizieren.
KW - Atherosclerosis
KW - Molecular imaging
KW - Elastin
KW - Plaque
KW - Interleukin-1beta
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610858
DO - https://doi.org/10.1038/s41598-024-71716-5
VL - 14
IS - 1
SP - 1
EP - 11
PB - Springer Science and Business Media LLC
AN - OPUS4-61085
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Nerger, Tino
A1 - Neumann, Patrick P.
A1 - Weller, Michael G.
T1 - Drone-Based Localization of Hazardous Chemicals by Passive Smart Dust
N2 - The distribution of tiny sensors over a specific area was first proposed in the late 1990s as a concept known as smart dust. Several efforts focused primarily on computing and networking capabilities, but quickly ran into problems related to power supply, cost, data transmission, and environmental pollution. To overcome these limitations, we propose using paper-based (confetti-like) chemosensors that exploit the inherent selectivity of chemical reagents, such as colorimetric indicators. In this work, cheap and biodegradable passive sensors made from cellulose could successfully indicate the presence of hazardous chemicals, e.g., strong acids, by a significant color change. A conventional color digital camera attached to a drone could easily detect this from a safe distance. The collected data were processed to define the hazardous area. Our work presents a combination of the smart dust concept, chemosensing, paper-based sensor technology, and low-cost drones for flexible, sensitive, economical, and rapid detection of hazardous chemicals in high-risk scenarios.
KW - Cellulose
KW - Passive Smart Dust
KW - Drohne
KW - Kolorimetrische Sensoren
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614641
DO - https://doi.org/10.3390/s24196195
VL - 24
IS - 19
SP - 1
EP - 16
PB - MDPI
AN - OPUS4-61464
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tscheuschner, Georg
A1 - Ponader, Marco
A1 - Raab, Christopher
A1 - Weider, Prisca S.
A1 - Hartfiel, Reni
A1 - Kaufmann, Jan Ole
A1 - Völzke, Jule L.
A1 - Bosc-Bierne, Gaby
A1 - Prinz, Carsten
A1 - Schwaar, T.
A1 - Andrle, Paul
A1 - Bäßler, Henriette
A1 - Nguyen, Khoa
A1 - Zhu, Y.
A1 - Mey, A. S. J. S.
A1 - Mostafa, A.
A1 - Bald, I.
A1 - Weller, Michael G.
T1 - Efficient Purification of Cowpea Chlorotic Mottle Virus by a Novel Peptide Aptamer
N2 - The cowpea chlorotic mottle virus (CCMV) is a plant virus explored as a nanotechnological platform. The robust self-assembly mechanism of its capsid protein allows for drug encapsulation and targeted delivery. Additionally, the capsid nanoparticle can be used as a programmable platform to display different molecular moieties. In view of future applications, efficient production and purification of plant viruses are key steps. In established protocols, the need for ultracentrifugation is a significant limitation due to cost, difficult scalability, and safety issues. In addition, the purity of the final virus isolate often remains unclear. Here, an advanced protocol for the purification of the CCMV from infected plant tissue was developed, focusing on efficiency, economy, and final purity. The protocol involves precipitation with PEG 8000, followed by affinity extraction using a novel peptide aptamer. The efficiency of the protocol was validated using size exclusion chromatography, MALDI-TOF mass spectrometry, reversed-phase HPLC, and sandwich immunoassay. Furthermore, it was demonstrated that the final eluate of the affinity column is of exceptional purity (98.4%) determined by HPLC and detection at 220 nm. The scale-up of our proposed method seems to be straightforward, which opens the way to the large-scale production of such nanomaterials. This highly improved protocol may facilitate the use and implementation of plant viruses as nanotechnological platforms for in vitro and in vivo applications.
N2 - Das Cowpea Chlorotic Mottle Virus (CCMV) ist ein Pflanzenvirus, das als nanotechnologische Plattform erforscht wird. Der robuste Selbstorganisationsmechanismus seines Kapsidproteins ermöglicht die Verkapselung und gezielte Abgabe von Medikamenten. Darüber hinaus kann das Kapsid-Nanopartikel als programmierbare Plattform für die Präsentation verschiedener molekularer Komponenten verwendet werden. Im Hinblick auf künftige Anwendungen ist eine effiziente Produktion und Reinigung von Pflanzenviren von entscheidender Bedeutung. In etablierten Protokollen stellt die notwendige Ultrazentrifugation aufgrund von Kosten, schwieriger Skalierbarkeit und Sicherheitsaspekten eine erhebliche Einschränkung dar. Darüber hinaus bleibt die Reinheit des endgültigen Virusisolats oft unklar. Hier wurde ein fortschrittliches Protokoll für die Reinigung von CCMV aus infiziertem Pflanzengewebe entwickelt, wobei der Schwerpunkt auf Effizienz, Wirtschaftlichkeit und Reinheit lag. Das Protokoll beinhaltet eine Fällung mit Polyethylenglycol (PEG 8000), gefolgt von einer Affinitätsextraktion mit einem neuartigen Peptid-Aptamer. Die Effizienz des Protokolls wurde mithilfe von Größenausschluss-Chromatographie (SEC), MALDI-TOF-Massenspektrometrie, Umkehrphasen-HPLC und Sandwich-Immunoassay validiert. Darüber hinaus wurde nachgewiesen, dass das endgültige Eluat der Affinitätssäule eine außergewöhnliche Reinheit (98,4 %) aufweist, die durch HPLC und Detektion bei 220 nm bestimmt wurde. Die Skalierung der von uns vorgeschlagenen Methode scheint einfach zu sein, was den Weg für eine größer angelegte Produktion solcher Nanomaterialien ebnet. Dieses stark verbesserte Protokoll könnte die Verwendung und Umsetzung von Pflanzenviren als nanotechnologische Plattformen für In-vitro- und In-vivo-Anwendungen erleichtern.
KW - Affinity chromatography
KW - Nanoparticles
KW - Nanoscience
KW - Carrier protein
KW - Encapsulation
KW - Combinatorial peptide library
KW - Peptide binder
KW - Vigna unguiculata
KW - Augenbohne
KW - Schlangenbohne
KW - Pflanzenvirus
KW - Plant virus
KW - Upscaling
KW - Commercialization
KW - Reference material
KW - Nanocarrier
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572645
DO - https://doi.org/10.3390/v15030697
VL - 15
IS - 3
SP - 1
EP - 24
PB - MDPI
CY - Basel, Schweiz
AN - OPUS4-57264
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Beslic, D.
A1 - Tscheuschner, Georg
A1 - Renard, B. Y.
A1 - Weller, Michael G.
A1 - Muth, Thilo
T1 - Comprehensive evaluation of peptide de novo sequencing tools for monoclonal antibody assembly
N2 - Monoclonal antibodies are biotechnologically produced proteins with various applications in research, therapeutics and diagnostics. Their ability to recognize and bind to specific molecule structures makes them essential research tools and therapeutic agents. Sequence information of antibodies is helpful for understanding antibody–antigen interactions and ensuring their affinity and specificity. De novo protein sequencing based on mass spectrometry is a valuable method to obtain the amino acid sequence of peptides and proteins without a priori knowledge. In this study, we evaluated six recently developed de novo peptide sequencing algorithms (Novor, pNovo 3, DeepNovo, SMSNet, PointNovo and Casanovo), which were not specifically designed for antibody data. We validated their ability to identify and assemble antibody sequences on three multi-enzymatic data sets. The deep learning-based tools Casanovo and PointNovo showed an increased peptide recall across different enzymes and data sets compared with spectrum-graph-based approaches. We evaluated different error types of de novo peptide sequencing tools and their performance for different numbers of missing cleavage sites, noisy spectra and peptides of various lengths. We achieved a sequence coverage of 97.69–99.53% on the light chains of three different antibody data sets using the de Bruijn assembler ALPS and the predictions from Casanovo. However, low sequence coverage and accuracy on the heavy chains demonstrate that complete de novo protein sequencing remains a challenging issue in proteomics that requires improved de novo error correction, alternative digestion strategies and hybrid approaches such as homology search to achieve high accuracy on long protein sequences.
KW - De novo peptide sequencing
KW - Bioinformatics
KW - Benchmarking study
KW - Monoclonal antibody
KW - Mass spectrometry
KW - Sequence coverage
KW - Light chains
KW - Heavy chains
KW - IgG
KW - Immunoglobulins
KW - Error correction
KW - Sequencing algorithm
KW - Preprocessing
KW - Missing fragmentation sites
KW - Deep learning-based tools
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570363
DO - https://doi.org/10.1093/bib/bbac542
VL - 24
IS - 1
SP - 1
EP - 12
PB - Oxford University Press
AN - OPUS4-57036
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fröhlich-Nowoisky, J.
A1 - Bothen, N.
A1 - Backes, A. T.
A1 - Weller, Michael G.
A1 - Pöschl, U.
T1 - Oligomerization and tyrosine nitration enhance the allergenic potential of the birch and grass pollen allergens Bet v 1 and Phl p 5
N2 - Protein modifications such as oligomerization and tyrosine nitration alter the immune response to allergens and may contribute to the increasing prevalence of allergic diseases. In this mini-review, we summarize and discuss relevant findings for the major birch and grass pollen allergens Bet v 1 and Phl p 5 modified with tetranitromethane (laboratory studies), peroxynitrite (physiological processes), and ozone and nitrogen dioxide environmental conditions). We focus on tyrosine nitration and the formation of protein dimers and higher oligomers via dityrosine cross-linking and the immunological effects studied.
N2 - Proteinmodifikationen wie Oligomerisierung und Tyrosinnitrierung verändern die Immunantwort auf Allergene und tragen möglicherweise zur zunehmenden Prävalenz allergischer Erkrankungen bei. In diesem Mini-Review fassen wir relevante Befunde zu den wichtigsten Birken- und Gräserpollenallergenen Bet v 1 und Phl p 5 zusammen, die mit Tetranitromethan (Laborstudien), Peroxynitrit (physiologische Prozesse) und Ozon und Stickstoffdioxid (Umweltbedingungen). Wir konzentrieren uns auf die Tyrosin-Nitrierung und die Bildung von Proteindimeren und höheren Oligomeren durch Dityrosin-Vernetzung und deren immunologischen Auswirkungen.
KW - Allergy
KW - Nitration
KW - Protein oligomers
KW - Air pollution
KW - Ozone
KW - Nitrogen oxides
KW - Tyrosine
KW - Nitrotyrosine
KW - Dityrosine
KW - Dityrosine crosslinking
KW - Protein degradation
KW - Neoepitopes
KW - Neoallergen
KW - IgE
KW - Immunoglobulin E
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591453
DO - https://doi.org/10.3389/falgy.2023.1303943
VL - 4
SP - 1
EP - 8
PB - Frontiers Media
CY - Switzerland
AN - OPUS4-59145
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Reinmuth-Selzle, K.
A1 - Bellinghausen, I.
A1 - Leifke, A. L.
A1 - Backes, A. T.
A1 - Bothen, N.
A1 - Ziegler, K.
A1 - Weller, Michael G.
A1 - Saloga, J.
A1 - Schuppan, D.
A1 - Lucas, K.
A1 - Pöschl, U.
A1 - Fröhlich-Nowoisky, J.
T1 - Chemical modification by peroxynitrite enhances TLR4 activation of the grass pollen allergen Phl p 5
N2 - The chemical modification of aeroallergens by reactive oxygen and nitrogen species (ROS/RNS) may contribute to the growing prevalence of respiratory allergies in industrialized countries. Post-translational modifications can alter the immunological properties of proteins, but the underlying mechanisms and effects are not well understood. In this study, we investigate the Toll-like receptor 4 (TLR4) activation of the major birch and grass pollen allergens Bet v 1 and Phl p 5, and how the physiological oxidant peroxynitrite (ONOO–) changes the TLR4 activation through protein nitration and the formation of protein dimers and higher oligomers. Of the two allergens, Bet v 1 exhibited no TLR4 activation, but we found TLR4 activation of Phl p 5, which increased after modification with ONOO– and may play a role in the sensitization against this grass pollen allergen. We attribute the TLR4 activation mainly to the two-domain structure of Phl p 5 which may promote TLR4 dimerization and activation. The enhanced TLR4 signaling of the modified allergen indicates that the ONOO–-induced modifications affect relevant protein-receptor interactions. This may lead to increased sensitization to the grass pollen allergen and thus contribute to the increasing prevalence of allergies in the Anthropocene, the present era of globally pervasive anthropogenic influence on the environment.
KW - Bet v 1
KW - Birch pollen allergen
KW - Phl p 5
KW - Grass pollen
KW - Phleum pratense
KW - Betula pendula
KW - Nitration
KW - Nitrotyrosine
KW - Protein nitration
KW - Toll-like receptor 4
KW - Allergy
KW - Enhancement
KW - Oligomerization
KW - Dimerization
KW - TLR4 activation
KW - Air pollution
KW - Nitrogen oxides
KW - Inflammation
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570298
DO - https://doi.org/10.3389/falgy.2023.1066392
VL - 4
SP - 1
EP - 7
PB - Frontiers Media SA
CY - Lausanne, Switzerland
AN - OPUS4-57029
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tchipilov, Teodor
A1 - Meyer, Klas
A1 - Weller, Michael G.
T1 - Quantitative 1H nuclear magnetic resonance (qNMR) of aromatic amino acids for protein quantification
N2 - Hydrolysis of protein samples into amino acids facilitates the use of NMR spectroscopy for protein and peptide quantification. Different conditions have been tested for quantifying aromatic amino acids and proteins. The pH-dependent signal shifts in the aromatic region of amino acid samples were examined. A pH of 12 was found to minimize signal overlap of the four aromatic amino acids. Several aromatic compounds, such as terephthalic acid, sulfoisophthalic acid, and benzene tricarboxylic acid, were applied as internal standards. The quantification of amino acids from an amino acid standard was performed. Using the first two suggested internal standards, recovery was ~97% for histidine, phenylalanine, and tyrosine at a concentration of approximately 1 mM in solution. Acidic hydrolysis of a certified reference material (CRM) of bovine serum albumin (BSA) and subsequent quantification of Phe and Tyr yielded recoveries of 98% ± 2% and 88% ± 4%, respectively, at a protein concentration of 16 g/L or 250 µM.
KW - Amino acid analysis
KW - Aromatic amino acid analysis
KW - AAA
KW - AAAA
KW - Protein hydrolysis
KW - Hydrochloric acid
KW - Metrology
KW - Traceability
KW - NIST
KW - Reference materials
KW - Internal standard
KW - Calibration
KW - Compound-independent calibration
KW - Histidine
KW - Tyrosine
KW - Tryptophan
KW - Phenylalanine
KW - Terephthalic acid
KW - Benzene-1,3,5-tricarboxylic acid
KW - Bovine serum albumin (BSA)
KW - Quantitative protein analysis
KW - Phenylketonuria
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570943
DO - https://doi.org/10.3390/mps6010011
VL - 6
IS - 1
SP - 1
EP - 13
PB - MDPI
CY - Basel, Schweiz
AN - OPUS4-57094
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Liu, Yanchen
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Montoro, Luciano A.
A1 - Liu, Hao
A1 - Liu, Ye
A1 - Emmerling, Franziska
A1 - Russo, Patrícia A.
A1 - Pinna, Nicola
T1 - A partially disordered crystallographic shear block structure as fast-charging negative electrode material for lithium-ion batteries
N2 - A well-ordered crystalline structure is crucial in battery electrodes, as the dimensionality and connectivity of the interstitial sites inherently influence Li+ ions diffusion kinetics. Niobium tungsten oxides block structures, composed of ReO3-type blocks of specific sizes with well-defined metal sites, are promising fast-charging negative electrode materials. Structural disorder is generally detrimental to conductivity or ion transport. However, here, we report an anomalous partially disordered Nb12WO33 structure that significantly enhances Li-ion storage performance compared to the known monoclinic Nb12WO33 phase. The partially disordered phase consists of corner-shared NbO6 octahedra blocks of varied sizes, including 5×4, 4×4, and 4×3, with a disordered arrangement of distorted WO4 tetrahedra at the corners of the blocks. This structural arrangement is robust during lithiation/delithiation, exhibiting minor local structure changes during cycling. It enables accelerated Li-ion migration, resulting in promising fast-charging performance, namely, 62.5 % and 44.7 % capacity retention at 20 C and 80 C, respectively. This study highlights the benefits of introducing disorder into niobium tungsten oxide shear structures, through the establishment of clear structure-performance correlations, offering guidelines for designing materials with targeted properties.
KW - Lithium ion batteries
KW - Oxides
KW - XANES
KW - XRD
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637994
DO - https://doi.org/10.1038/s41467-025-61646-9
SN - 2041-1723
VL - 16
IS - 1
SP - 1
EP - 15
PB - Springer Science and Business Media LLC
AN - OPUS4-63799
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heinekamp, Christian
A1 - Roy, Arkendu
A1 - Karafiludis, Stephanos
A1 - Kumar, Sourabh
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Stawski, Tomasz M.
A1 - Miliūtė, Aistė
A1 - von der Au, Marcus
A1 - Ahrens, Mike
A1 - Braun, Thomas
A1 - Emmerling, Franziska
T1 - Zirconium fluoride-supported high-entropy fluoride: a catalyst for enhanced oxygen evolution reaction
N2 - Extended hydrogen initiatives promote the urgency of research on water splitting technologies and, therein, oxygen evolution reaction catalysts being developed. A route to access a ZrF4 supported high-entropy fluoride catalyst using a facile sol–gel route is presented. The high-entropy character of the catalyst was confirmed by scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDX) as well as inductively coupled plasma-mass spectrometry (ICP-MS). Additional investigations on the local structure were performed using extended X-ray absorption fine structure spectroscopy (EXAFS) and pair distribution function (PDF) analysis. The catalyst shows significant potential for oxygen evolution reaction (OER) in alkaline media with a current density of 100 mA cm−2 at approximately 1.60 V, thus outperforming benchmark materials such as IrO2, despite a significant reduction in electrochemical mass loading. A potential mechanism is suggested based on free energy calculation using DFT calculations.
KW - OER
KW - HEA
KW - CCMAT
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637116
DO - https://doi.org/10.1039/D4TA08664C
SN - 2050-7488
VL - 13
IS - 26
SP - 20383
EP - 20393
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-63711
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dittmar, Stefan
A1 - Weyrauch, Steffen
A1 - Reemtsma, Thorsten
A1 - Eisentraut, Paul
A1 - Altmann, Korinna
A1 - Ruhl, Aki S.
A1 - Jekel, Martin
T1 - Settling Velocities of Tire and Road Wear Particles: Analyzing Finely Graded Density Fractions of Samples from a Road Simulator and a Highway Tunnel
N2 - The terminal settling velocity is considered the most critical parameter determining the transport of tire and road wear particles (TRWP) in aquatic environments. Nonetheless, no respective empirical data has been reported so far. In this study, particle samples from a road simulator and a highway tunnel were investigated with a validated imaging method. Different density and size fractions of both samples were measured separately, acquiring sizes and settling velocities of more than 30,000 individual particles. In addition, tire marker polymers were analyzed for each fraction via thermal extraction desorption-gas chromatography/mass spectrometry. Finally, the acquired particle data was combined according to the fractions’ estimated tire contents in order to deduce detailed probability distributions of particle size and settling velocity for the actual TRWP from both samples. Weighted by TRWP-incorporated tire mass, median diameters of 54 and 44 μm as well as median settling velocities of 0.65 and 0.22 mm/s were found for TRWP from the road simulator and highway tunnel, respectively. This study thus provides the first ever empirical data on TRWP settling velocities in water, which can be highly valuable input for modeling the environmental transport of TRWP and for dimensioning TRWP retention systems.
KW - Microplastics
KW - TED-GC/MS
KW - Sinking velocities
KW - Transport
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635449
DO - https://doi.org/10.1021/acs.est.5c04165
SN - 0013-936X
VL - 59
IS - 26
SP - 13434
EP - 13446
PB - American Chemical Society (ACS)
AN - OPUS4-63544
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Das, Prasenjit
A1 - Chakraborty, Gouri
A1 - Yang, Jin
A1 - Roeser, Jérôme
A1 - Küçükkeçeci, Hüseyin
A1 - Nguyen, Anh Dung
A1 - Schwarze, Michael
A1 - Gabriel, Jose
A1 - Penschke, Christopher
A1 - Du, Shengjun
A1 - Weigelt, Vincent
A1 - Khalil, Islam E.
A1 - Schmidt, Johannes
A1 - Saalfrank, Peter
A1 - Oschatz, Martin
A1 - Rabeah, Jabor
A1 - Schomäcker, Reinhard
A1 - Emmerling, Franziska
A1 - Thomas, Arne
T1 - The Effect of Pore Functionality in Multicomponent Covalent Organic Frameworks on Stable Long‐Term Photocatalytic H2 Production
N2 - AbstractIn nature, organic molecules play a vital role in light harvesting and photosynthesis. However, regarding artificial water splitting, the research focus is primarily on inorganic semiconductors. Although organic photocatalysts have high structural variability, they tend to exhibit lower quantum efficiencies for water splitting than their inorganic counterparts. Multicomponent reactions (MCRs) offer an attractive route to introduce different functional units into covalent organic frameworks (COFs) and enable semiconducting properties and high chemical stability, creating promising materials for long‐term photocatalytic applications, such as H2 production. Herein, five highly crystalline donor‐acceptor based, 4‐substituted quinoline‐linked MCR‐COFs are presented that are prepared via the three‐component Povarov reaction. The pore functionality is varied by applying different vinyl derivatives (e.g., styrene, 2‐vinyl pyridine, 4‐vinylpyridine, 4‐vinyl imidazole, 2,3,4,5,6‐pentafluorostyrene), which has a strong influence on the obtained photocatalytic activity. Especially an imidazole‐functionalized COF displays promising photocatalytic performance due to its high surface area, crystallinity, and wettability. These properties enable it to maintain its photocatalytic activity even in a membrane support. Furthermore, such MCR‐COFs display dramatically enhanced (photo)chemical stability even after long‐term solar light irradiation and exhibit a high and steady H2 evolution for at least 15 days.
KW - Sstability
KW - Covalent organic frameworks
KW - Pore functionality
KW - Long-term H2 production
KW - Multicomponent reactions
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639787
DO - https://doi.org/10.1002/aenm.202501193
SN - 1614-6832
SP - 1
EP - 10
PB - Wiley VHC-Verlag
AN - OPUS4-63978
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Visileanu, Emilia
A1 - Altmann, Korinna
A1 - Stepa, Raluca
A1 - Haiducu, Maria
A1 - Miclea, Paul Tiberiu
A1 - Vladu, Alina
A1 - Dondea, Felicia
A1 - Grosu, Marian Catalin
A1 - Scarlat, Razvan
T1 - Comparative Analysis of Airborne Particle Concentrations in Textile Industry Environments Throughout the Workday
N2 - This paper addresses the growing concern surrounding microplastic pollution, particularly within the textile industry, and the associated potential health risks linked to the inhalation and ingestion of microplastic particles. Microplastics, defined as plastic particles smaller than five millimeters, are increasingly found not only in aquatic environments, but also in soils, air, and food. Although research on the health impacts of microplastics is still emerging, early studies indicate that these particles could contribute to health issues, including oxidative stress, inflammation, and cardiovascular diseases. Notably, individuals with higher concentrations of plastics in arterial plaques are more susceptible to heart attacks and strokes. In the textile industry, synthetic fibers such as polyester, nylon, and acrylic release microplastics into the air during production. The paper discusses a study conducted in a textile company that processes polyester yarns, where airborne microplastic concentrations were measured at various locations throughout the day. Particle sizes ranging from 0.3 nm to 10 nm were analyzed, revealing the presence of polyester polymers in the particulate matter. These findings underscore the widespread nature of microplastic pollution, particularly in industrial settings, and raise concerns about the health risks associated with prolonged exposure to airborne microplastics. While further research is necessary to fully understand the extent of these health impacts, preliminary data suggest a troubling link between microplastic inhalation and cardiovascular conditions.
KW - Microplastics
KW - Textiles
KW - Airborne particles
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635269
DO - https://doi.org/10.3390/microplastics4020034
SN - 2673-8929
VL - 4
IS - 2
SP - 1
EP - 17
PB - MDPI AG
AN - OPUS4-63526
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez-Sánchez, Noelia
A1 - Domínguez-Santos, J. Enrique
A1 - Bhattacharya, Biswajit
A1 - Prinz, Carsten
A1 - Canosa, Inés
A1 - Flores, Amando
A1 - Jiménez-Rodríguez, Antonia
A1 - Ruiz-Salvador, A. Rabdel
A1 - Emmerling, Franziska
A1 - Ballesteros, Menta
T1 - Mechanochemical synthesis of multivariate UPO-3 (Cu-ZIF-9-ica) MOF for inactivation of antibiotic-resistant bacteria and irrigation-quality water production via heterogeneous photo-Fenton catalysis
N2 - Water scarcity and pollution are critical global challenges, particularly in agriculture, the largest consumer of water. The development of sustainable, effective, and environmentally friendly disinfection methods is essential to address the risks posed by antibiotic-resistant bacteria and to ensure safe reuse of water for irrigation. In this study, we report the synthesis of the metal-organic framework (MOF) Universidad Pablo de Olavide-3 (UPO-3) via a mechanochemical approach, a scalable and sustainable method compared to traditional solvothermal synthesis. The resulting UPO-3/H2O2 system exhibits robust photocatalytic properties under visible light, achieving effective and broad-spectrum antibacterial activity. The disinfection efficiency of the catalyst was evaluated against Escherichia coli as a model of microbial pathogen in two saline matrices, considering the key parameters of the heterogeneous photo-Fenton process, including catalyst dosage, initial H2O2 concentration, and light irradiation. Notably, it inactivated two important virulent and antibiotic-resistant bacterial pathogens (Staphylococcus aureus and Pseudomonas aeruginosa). Furthermore, UPO-3 shows exceptional performance under real-world conditions, such as river water disinfection, achieving >5-log reduction of E. coli, fulfilling a critical criterion for Class A water reuse under Regulation (EU) 2020/741. These results highlight UPO-3 as a versatile and sustainable solution for water reuse, addressing water scarcity and advancing efforts to achieve United Nations Sustainable Development Goal 6.
KW - Water reuse
KW - Antibiotic-resistant bacteria
KW - Water disinfection
KW - Mechanochemical synthesis
KW - Metal organic framework
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639766
DO - https://doi.org/10.1016/j.chemosphere.2025.144610
SN - 0045-6535
VL - 386
SP - 1
EP - 11
PB - Elsevier Ltd.
AN - OPUS4-63976
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Go, Eun Sul
A1 - Hong, Eun Ji
A1 - Lee, Ji Yeong
A1 - Stolar, Tomislav
A1 - Peterson, Gregory I.
A1 - Emmerling, Franziska
A1 - Kim, Kyoungsoo
A1 - Kim, Jeung Gon
T1 - Insights into Mechanochemical Solid-State Ball-Milling Reaction: Monitoring Transition from Heterogeneous to Homogeneous Conditions
N2 - As mechanochemical synthesis has advanced significantly, there has been intense interest in understanding the underlying mechanisms of these reactions. Given that many mechanochemical processes are conducted in the solid-state without solvation yet sometimes yield faster reactions than those in solution, we sought to address the following question: Are mechanochemical reactions homo- or heterogeneous? To investigate, we employed a model system involving the mixing and copolymerization of l-lactide (LLA) and d-lactide (DLA), monitored through powder X-ray diffraction (PXRD), nuclear magnetic resonance, and differential scanning calorimetry. In situ and ex situ PXRD analyses of the mixture of LLA and DLA showed that vibratory ball milling rapidly transformed the initially heterogeneous lactide mixture into a homogeneous phase within one min due to collisions between the balls and the jar. By varying the milling conditions, we were able to regulate the level of mixing, which subsequently influenced the copolymerization outcomes. In the solid-state ball-milling copolymerization of LLA and DLA in the presence of a catalyst and initiator, multiblock copolymers of poly(l-lactic acid) and poly(d-lactic acid) were formed within one min during the early stage of the reaction, when incomplete mixing of the monomers led to a process governed by phase heterogeneity. In contrast, prolonged polymerization promoted conditions approaching homogeneity, ultimately yielding atactic poly(lactic acid). This transition from heterogeneous to homogeneous reactions is a distinctive feature compared to conventional homogeneous reactions, potentially leading to mechano-exclusive reaction designs.
KW - Mechanochemistry
KW - Ball-milling
KW - Homogeneous reaction
KW - Heterogeneous reaction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638008
DO - https://doi.org/10.1021/jacsau.5c00322
SN - 2691-3704
VL - 5
IS - 6
SP - 2720
EP - 2727
PB - American Chemical Society (ACS)
AN - OPUS4-63800
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Feiler, Torvid
A1 - Emmerling, Franziska
A1 - Bhattacharya, Biswajit
T1 - Sustainable mechanochemical approach for the selective synthesis of multicomponent organic solids: real-time in situ insights
N2 - Crystalline multicomponent organic solids (MOSs) such as cocrystals and ionic cocrystals hold immense potential in diverse functional applications, ranging from pharmaceuticals to optoelectronics. However, conventional solution-based crystallization methods often result in polymorphic mixtures and lack precise control over product composition. Herein, we report a comparative investigation of solution crystallization versus mechanochemical synthesis for constructing MOSs from 9-anthracenecarboxylic acid (ACA) and 4,4 '-bipyridine (BPY). Solution-based approaches consistently yielded concomitant formation of neutral cocrystal (CC) and ionic cocrystal (ICC) forms, regardless of the solvent used. The resulting multicomponent solids were comprehensively characterized using a combination of single crystal X-ray diffraction, powder X-ray diffraction, Fourier-transform infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. In contrast, mechanochemical methods, including neat grinding (without solvent) and liquid-assisted grinding (with minimum solvent), enabled selective formation of either a phase pure CC or ICC form. Less polar and nonpolar organic solvents favor the kinetic CC, while polar water promotes formation of the thermodynamically stable ICC. Time-resolved in situ powder X-ray diffraction (TRIS-PXRD) captures the dynamic evolution of solid-state phases and reveals the complete transformation of the CC into ICC under neat grinding or water-assisted conditions. This study highlights the powerful role of mechanochemistry and in situ monitoring in steering solid-state reactivity and offers a sustainable pathway for the targeted and scalable synthesis of pure multicomponent organic materials.
KW - Cocrystal
KW - Synchrotron X-ray powder diffraction
KW - Time-resolved in situ investigation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641409
DO - https://doi.org/10.1039/D5CE00663E
SN - 1466-8033
SP - 1
EP - 9
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64140
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Karafiludis, Stephanos
A1 - Scoppola, E.
A1 - Wolf, S.E.
A1 - Kochovski, Z.
A1 - Matzdorff, D.
A1 - Van Driessche, A. E. S.
A1 - Hövelmann, J.
A1 - Emmerling, Franziska
A1 - Stawski, Tomasz M.
T1 - Evidence for liquid-liquid phase separation during the early stages of Mg-struvite formation
N2 - The precipitation of struvite, a magnesium ammonium phosphate hexahydrate (MgNH₄PO₄ · 6H₂O) mineral, from wastewater is a promising method for recovering phosphorous. While this process is commonly used in engineered environments, our understanding of the underlying mechanisms responsible for the formation of struvite crystals remains limited. Specifically, indirect evidence suggests the involvement of an amorphous precursor and the occurrence of multi-step processes in struvite formation, which would indicate non-classical paths of nucleation and crystallization. In this study, we use synchrotron-based in situ x-ray scattering complemented by cryogenic transmission electron microscopy to obtain new insights from the earliest stages of struvite formation. The holistic scattering data captured the structure of an entire assembly in a time-resolved manner. The structural features comprise the aqueous medium, the growing struvite crystals, and any potential heterogeneities or complex entities. By analysing the scattering data, we found that the onset of crystallization causes a perturbation in the structure of the surrounding aqueous medium. This perturbation is characterized by the occurrence and evolution of Ornstein-Zernike fluctuations on a scale of about 1 nm, suggesting a non-classical nature of the system. We interpret this phenomenon as a liquid-liquid phase separation, which gives rise to the formation of the amorphous precursor phase preceding actual crystal growth of struvite. Our microscopy results confirm that the formation of Mg-struvite includes a short-lived amorphous phase, lasting >10 s.
KW - Physical and theoretical chemistry
KW - Non-classical crystallization
KW - Struvite
KW - Liquid-liquid-phase-separation
KW - Nucleation
KW - Crystallization
KW - In-situ scattering
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584766
DO - https://doi.org/10.1063/5.0166278
SN - 1089-7690
VL - 159
IS - 13
SP - 1
EP - 12
PB - AIP Publishing
CY - Woodbury, NY
AN - OPUS4-58476
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stawski, Tomasz
A1 - Karafiludis, Stephanos
A1 - Pimentel, Carlos
A1 - Montes-Hernández, German
A1 - Kochovski, Zdravko
A1 - Bienert, Ralf
A1 - Weimann, Karin
A1 - Emmerling, Franziska
A1 - Scoppola, Ernesto
A1 - Van Driessche, Alexander E.S.
T1 - Solution-driven processing of calcium sulfate: The mechanism of the reversible transformation of gypsum to bassanite in brines
N2 - Here, we show that calcium sulfate dihydrate (gypsum) can be directly, rapidly and reversibly converted to calcium sulfate hemihydrate (bassanite) in high salinity solutions (brines). The optimum conditions for the efficient production of bassanite in a short time (<5 min) involve the use of brines with c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the better-known behaviour of the bassanite phase in low-salt environments. In low-salinity aqueous solutions, bassanite is considered to be metastable with respect to gypsum and anhydrite, and therefore gypsum-to-bassanite conversion does not occur in pure water. Interestingly, the high-salinity transformation of gypsum-to-bassanite has been reported by many authors and used in practice for several decades, although its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures was inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline phase for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios.
KW - Industrial and Manufacturing Engineering
KW - Strategy and Management
KW - General Environmental Science
KW - Renewable Energy, Sustainability and the Environment
KW - Building and Construction
KW - Calcium sulfate
KW - Gypsum
KW - Bassanite
KW - Scattering
KW - Raman
KW - In situ
KW - Synchrotron
KW - BESSY
KW - MySpot
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594698
UR - https://www.sciencedirect.com/science/article/pii/S0959652624004591#appsec1
DO - https://doi.org/10.1016/j.jclepro.2024.141012
SN - 0959-6526
VL - 440
SP - 1
EP - 12
PB - Elsevier B.V.
AN - OPUS4-59469
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Edzards, Joshua
A1 - Saßnick, Holger-Dietrich
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Valencia, Ana M.
A1 - Emmerling, Franziska
A1 - Beyer, Sebastian
A1 - Cocchi, Caterina
T1 - Effects of Ligand Substituents on the Character of Zn-Coordination in Zeolitic Imidazolate Frameworks
N2 - Due to their favorable properties and high porosity, zeolitic imidazolate frameworks (ZIFs) have recently received much limelight for key technologies such as energy storage, optoelectronics, sensorics, and catalysis. Despite widespread interest in these materials, fundamental questions regarding the zinc coordination environment remain poorly understood. By focusing on zinc(II)2-methylimidazolate (ZIF-8) and its tetrahedrally coordinated analogues with Br-, Cl-, and H-substitution in the 2-ring position, we aim to clarify how variations in the local environment of Zn impact the charge distribution and the electronic properties of these materials. Our results from densityfunctional theory confirm the presence of a Zn coordinative bond with a large polarization that is quantitatively affected by different substituents on the organic ligand. Moreover, our findings suggest that the variations in the Zn coordination induced by the functionalization have a negligible effect on the electronic structure of the considered compounds. On the other hand, halogen terminations of the ligands lead to distinct electronic contributions in the vicinity of the frontier region which ultimately reduce the band gap size by a few hundred millielectron volts. Experimental results obtained from X-ray absorption spectroscopy (Zn K-edge) confirm the trends predicted by theory and, together with them, contribute to a better understanding of the structure−property relationships that are needed to tailor ZIFs for target applications.
KW - Surfaces
KW - Physical and Theoretical Chemistry
KW - General Energy
KW - Electronic
KW - Coatings and Films
KW - Optical and Magnetic Materials
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589117
DO - https://doi.org/10.1021/acs.jpcc.3c06054
SN - 1932-7447
VL - 127
IS - 43
SP - 21456
EP - 21464
PB - American Chemical Society (ACS)
AN - OPUS4-58911
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zuffa, Caterina
A1 - Cappuccino, Chiara
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Maini, Lucia
T1 - Liquid reagents are not enough for liquid assisted grinding in the synthesis of [(AgBr)(n-pica)]n
N2 - This study investigates the mechanochemical reactions between AgBr 3-picolylamine and 4-picolylamine. The use of different stoichiometry ratios of the reagents allows [(AgBr)(n-pica)]n and [(AgBr)2(n-pica)]n to be obtained, and we report the new structures of [(AgBr)2(3-pica)]n and [(AgBr)2(4-pica)]n which are characterized by the presence of the following: (a) infinite inorganic chains, (b) silver atom coordinated only by bromide atoms and (c) argentophilic interactions. Furthermore, we studied the interconversion of [(AgBr)(n-pica)]n/[(AgBr)2(n-pica)]n by mechanochemical and thermal properties. The in situ experiments suggest that [(AgBr)(3-pica)]n is kinetically favoured while [(AgBr)2(3-pica)]n is converted into [(AgBr)(3-pica)]n only with a high excess of the ligand. Finally, the liquid nature of the ligands is not sufficient to assist the grinding process, and the complete reaction is observed with the addition of a small quantity of acetonitrile.
KW - Mechanochemistry
KW - Complex
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594755
DO - https://doi.org/10.1039/d3cp04791a
SN - 1463-9076
SP - 1
EP - 10
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59475
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Villajos Collado, José Antonio
A1 - Bienert, M.
A1 - Gugin, Nikita
A1 - Emmerling, Franziska
A1 - Maiwald, Michael
T1 - A database to select affordable MOFs for volumetric hydrogen cryoadsorption considering the cost of their linkers
N2 - Physical adsorption at cryogenic temperature (cryoadsorption) is a reversible mechanism that can reduce the pressure of conventional compressed gas storage systems. Metal–organic framework (MOF) materials are remarkable candidates due to the combination of high specific surface area and density which, in some cases, provide a high volumetric storage capacity. However, such extensive use of MOFs for this application requires the selection of affordable structures, easy to produce and made from feasible metallic and organic components. Herein, we introduce a MOF database detailing the crystallographic and porous properties of 3600 existing MOFs made from industrially relevant metals and their organic composition. The comparison of the available minimum costs of linkers allowed the creation of a database to select affordable structures with high potential for volumetric hydrogen storage by cryoadsorption, considering their composition based on individual or mixed building blocks. A user inter� face, available online, facilitates the selection of MOFs based on the properties or names of structures and linkers.
KW - MOF´s
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583619
DO - https://doi.org/10.1039/d3ma00315a
VL - 4
IS - 18
SP - 4226
EP - 4237
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58361
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scheurrell, Kerstin
A1 - B. Martins, Inês C.
A1 - Murray, Claire
A1 - Emmerling, Franziska
T1 - Exploring the role of solvent polarity in mechanochemical Knoevenagel condensation: in situ investigation and isolation of reaction intermediates
N2 - Mechanochemistry has proven to be a highly effective method for the synthesis of organic compounds. We studied the kinetics of the catalyst-free Knoevenagel reaction between 4-nitrobenzaldehyde and malononitrile, activated and driven by ball milling. The reaction was investigated in the absence of solvents (neat grinding) and in the presence of solvents with different polarities (liquid-assisted grinding). The reaction was monitored using time-resolved in situ Raman spectroscopy and powder X-ray diffraction (PXRD). Our results indicate a direct relationship between solvent polarity and reaction kinetics, with higher solvent polarity leading to faster product (2-(4-nitrobenzylidone)malononitrile) formation. For the first time, we were able to isolate and determine the structure of an intermediate 2-(hydroxy(4-nitrophenyl)methyl)malononitrile based on PXRD data.
KW - Physical and Theoretical Chemistry
KW - General Physics and Astronomy
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588071
DO - https://doi.org/10.1039/D3CP02883F
SN - 1463-9076
VL - 25
IS - 35
SP - 23637
EP - 23644
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58807
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Peters, Stefan
A1 - Kunkel, Benny
A1 - Cakir, Cafer Tufan
A1 - Kabelitz, Anke
A1 - Witte, Steffen
A1 - Bernstein, Thomas
A1 - Bartling, Stephan
A1 - Radtke, Martin
A1 - Emmerling, Franziska
A1 - Abdel-Mageed, Ali Mohamed
A1 - Wohlrab, Sebastian
A1 - de Oliveira Guilherme Buzanich, Ana
T1 - Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy
N2 - A novel setup for dispersive X-ray absorption spectroscopy (XAS) with simultaneous resolution of space, time and energy for in situ characterization of solid materials is demonstrated.
KW - Dispersive XAS
KW - Catalysis
KW - In situ
KW - Structure analysis
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584924
DO - https://doi.org/10.1039/d3cc03277a
SN - 1359-7345
SP - 1
EP - 4
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58492
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wiesner, Yosri
A1 - Bednarz, Marius
A1 - Braun, Ulrike
A1 - Bannick, Claus Gerhard
A1 - Ricking, Mathias
A1 - Altmann, Korinna
T1 - A promising approach to monitor microplastic masses in composts
N2 - Inputs of plastic impurities into the environment via the application of fertilizers are regulated in Germany and the EU by means of ordinances. Robust and fast analytical methods are the basis of legal regulations. Currently, only macro- and large microplastic contents (>1 mm) are measured. Microplastics (1–1,000 µm), are not yet monitored. Thermal analytical methods are suitable for this purpose, which can determine the mass content and can also be operated fully automatically in routine mode. Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) allows the identification of polymers and the determination of mass contents in solid samples from natural environments. In accordance with the German or European Commission (EC) Fertiliser Ordinance, composting plants should be monitored for microplastic particles with this method in the future. In this context a compost plant was sampled. At the end of the rotting process, the compost was sieved and separated in a coarse (>1 mm) and a fine fraction (<1 mm). The fine fraction was processed using density separation comparing NaCl and NaI as possible salt alternative and screened for microplastic masses by TED-GC/MS with additional validation and quality assurance experiments. With TED-GC/MS total microplastics mass contents of 1.1–3.0 μg/mg in finished compost could be detected with polyethylene mainly. What differs much to the total mass of plastics in the coarse fraction with up to 60 μg/mg, which were visually searched, identified via ATR-FTIR and gravimetrically weighted.
KW - Microplastics
KW - TED-GC/MS
KW - Compost
KW - Monitoring
KW - Soil
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586688
DO - https://doi.org/10.3389/fenvc.2023.1281558
SN - 2673-4486
VL - 4
SP - 1
EP - 12
PB - Frontiers Media
CY - Lausanne
AN - OPUS4-58668
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heinekamp, Christian
A1 - Kneiske, Sönke
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Ahrens, Mike
A1 - Braun, Thomas
A1 - Emmerling, Franziska
T1 - A fluorolytic sol-gel route to access an amorphous Zr fluoride catalyst: A useful tool for C-F bond activation
N2 - A route to a ZrF4 catalyst active in room temperature Friedel–Crafts and dehydrofluorination reactions was developed via a fluorolytic sol–gel route, which was followed by a postfluorination step using a stream of CHClF2. The behaviour of different Zr(IV) precursors in a sol–gel reaction with anhydrous isopropanol/HF solution was investigated. The subsequent post-fluorination step was optimised in its temperature ramp and confirmed the necessity of a fluorination of the generated xerogels to obtain catalytic activity. The process is discussed in the context of the analysis of the materials using Brunauer–Emmett–Teller analysis (BET), powder X-ray diffraction (XRD), infrared spectroscopy (IR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The local structure of the amorphous catalyst was elucidated by extended X-ray absorption fine structure spectroscopy (EXAFS).
KW - Catalysis
KW - Heterogeneous catalysis
KW - C-F bond activation
KW - Postfluorination
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593433
DO - https://doi.org/10.1039/D3CY01439H
SN - 2044-4761
SP - 1
EP - 8
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59343
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Paul, Martin
A1 - Tscheuschner, Georg
A1 - Herrmann, Stefan
A1 - Weller, Michael G.
T1 - Fast Detection of 2,4,6-Trinitrotoluene (TNT) at ppt Level by a Laser-Induced Immunofluorometric Biosensor
N2 - The illegal use of explosives by terrorists and other criminals is an increasing issue in public spaces, such as airports, railway stations, highways, sports venues, theaters, and other large buildings. Security in these environments can be achieved by different means, including the installation of scanners and other analytical devices to detect ultra-small traces of explosives in a very short time-frame to be able to take action as early as possible to prevent the detonation of such devices. Unfortunately, an ideal explosive detection system still does not exist, which means that a compromise is needed in practice. Most detection devices lack the extreme analytical sensitivity, which is nevertheless necessary due to the low vapor pressure of nearly all explosives. In addition, the rate of false positives needs to be virtually zero, which is also very difficult to achieve. Here we present an immunosensor system based on kinetic competition, which is known to be very fast and may even overcome affinity limitation, which impairs the performance of many traditional competitive assays. This immunosensor consists of a monolithic glass column with a vast excess of immobilized hapten, which traps the fluorescently labeled antibody as long as no explosive is present. In the case of the explosive 2,4,6-trinitrotoluene (TNT), some binding sites of the antibody will be blocked, which leads to an immediate breakthrough of the labeled protein, detectable by highly sensitive laser-induced fluorescence with the help of a Peltier-cooled complementary metal-oxide-semiconductor (CMOS) camera. Liquid handling is performed with high-precision syringe pumps and chip-based mixing-devices and flow-cells. The system achieved limits of detection of 1 pM (1 ppt) of the fluorescent label and around 100 pM (20 ppt) of TNT. The total assay time is less than 8 min. A cross-reactivity test with 5000 pM solutions showed no signal by pentaerythritol tetranitrate (PETN), 1,3,5-trinitroperhydro-1,3,5-triazine (RDX), and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX). This immunosensor belongs to the most sensitive and fastest detectors for TNT with no significant cross-reactivity by non-related compounds. The consumption of the labeled antibody is surprisingly low: 1 mg of the reagent would be sufficient for more than one year of continuous biosensor operation.
KW - Airport
KW - Aviation
KW - Bombs
KW - Terrorism
KW - Biosensing
KW - Continuous Sensor
KW - High-Speed
KW - Ultrasensitive
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511245
DO - https://doi.org/10.3390/bios10080089
VL - 10
IS - 8
SP - 89
PB - MDPI
CY - Basel
AN - OPUS4-51124
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Costa, Elena
A1 - Climent Terol, Estela
A1 - Gawlitza, Kornelia
A1 - Wan, Wei
A1 - Weller, Michael G.
A1 - Rurack, Knut
T1 - Optimization of analytical assay performance of antibody-gated indicator-releasing mesoporous silica particles
N2 - Antibody-gated indicator delivery (gAID) systems based on mesoporous silica nano- and microparticle scaffolds are a promising class of materials for the sensitive chemical detection of small-molecule analytes in simple test formats such as lateral flow assays (LFAs) or microfluidic chips. Their architecture is reminiscent of drug delivery systems, only that reporter molecules instead of drugs are stored in the voids of a porous host particle. In addition, the pores are closed with macromolecular “caps” through a tailored “gatekeeping” recognition chemistry so that the caps are opened when an analyte has reacted with a “gatekeeper”. The subsequent uncapping leads to a release of a large number of indicator molecules, endowing the system with signal amplification features. Particular benefits of such systems are their modularity and adaptability. With the example of the immunochemical detection of type-I pyrethroids by fluorescent dye-releasing gAID systems, the influence of several tuning modes on the optimisation of such hybrid sensory materials is introduced here. In particular, different mesoporous silica supports (from nano- and microparticles to platelets and short fibres), different functionalisation routes and different loading sequences were assessed. The materials’ performances were evaluated by studying their temporal response behaviour and detection sensitivity, including the tightness of pore closure (through the amount of blank release in the absence of analyte) and the release kinetics. Our results indicate that the better the paratope-accommodating Fab region of the antibody “cap” fits into the host material's pore opening, the better the closing/opening mechanism can be controlled. Because such materials are well-suited for LFAs, performance assessment included a test-strip format besides conventional assays in suspension. In combination with dyes as indicators and smartphones for read-out, simple analytical tests for use by untrained personnel directly at a point-of-need such as an aeroplane cabin can be devised, allowing for sensitivities down to the μg kg−1 range in <5 min with case-required selectivities.
KW - Antibody-gated indicator delivery
KW - Lateral flow assay
KW - SBA-15
KW - SBA-16
KW - Type-I pyrethroids
KW - Phenothrin
KW - Permethrin
KW - Etofenprox
KW - Amplification
KW - Biosensors
KW - Immunoassays
KW - Mesoporous particles
KW - Optical detection
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517053
DO - https://doi.org/10.1039/d0tb00371a
VL - 8
IS - 22
SP - 4950
EP - 4961
PB - Royal Society of Chemistry
AN - OPUS4-51705
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tscheuschner, Georg
A1 - Schwaar, Timm
A1 - Weller, Michael G.
T1 - Fast Confirmation of Antibody Identity by MALDI-TOF MS Fingerprints
N2 - Thousands of antibodies for diagnostic and other analytical purposes are on the market. However, it is often difficult to identify duplicates, reagent changes, and to assign the correct original publications to an antibody. This slows down scientific progress and might even be a cause of irreproducible research and a waste of resources. Recently, activities were started to suggest the sole use of recombinant antibodies in combination with the open communication of their sequence. In this case, such uncertainties should be eliminated. Unfortunately, this approach seems to be rather a long-term vision since the development and manufacturing of recombinant antibodies remain quite expensive in the foreseeable future. Nearly all commercial antibody suppliers also may be reluctant to publish the sequence of their antibodies, since they fear counterfeiting. De novo sequencing of antibodies is also not feasible today for a reagent user without access to the hybridoma clone. Nevertheless, it seems to be crucial for any scientist to have the opportunity to identify an antibody undoubtedly to guarantee the traceability of any research activity using antibodies from a third party as a tool. For this purpose, we developed a method for the identification of antibodies based on a MALDI-TOF MS fingerprint. To circumvent lengthy denaturation, reduction, alkylation, and enzymatic digestion steps, the fragmentation was performed with a simple formic acid hydrolysis step. Eighty-nine unknown monoclonal antibodies were used for this study to examine the feasibility of this approach. Although the molecular assignment of peaks was rarely possible, antibodies could be easily recognized in a blinded test, simply from their mass-spectral fingerprint. A general protocol is given, which could be used without any optimization to generate fingerprints for a database. We want to propose that, in most scientific projects relying critically on antibody reagents, such a fingerprint should be established to prove and document the identity of the used antibodies, as well as to assign a specific reagent to a datasheet of a commercial supplier, public database record, or antibody ID.
KW - Reproducibility
KW - Quality Control
KW - Traceability
KW - Diagnostics
KW - Hybridoma
KW - Monoclonal Antibody
KW - Recombinant Antibody
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506611
DO - https://doi.org/10.3390/antib9020008
SN - 2073-4468
VL - 9
IS - 2
SP - 1
EP - 17
PB - MDPI
CY - Basel
AN - OPUS4-50661
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ziegler, K.
A1 - Kunert, A. T.
A1 - Reinmuth-Selzle, K.
A1 - Leifke, A. L.
A1 - Widera, D.
A1 - Weller, Michael G.
A1 - Schuppan, D.
A1 - Fröhlich-Nowoisky, J.
A1 - Lucas, K.
A1 - Pöschl, U.
T1 - Chemical modification of pro-inflammatory proteins by peroxynitrite increases activation of TLR4 and NF-κB: Implications for the health effects of air pollution and oxidative stress
N2 - Environmental pollutants like fine particulate matter can cause adverse health effects through oxidative stress and inflammation. Reactive oxygen and nitrogen species (ROS/RNS) such as peroxynitrite can chemically modify proteins, but the effects of such modifications on the immune system and human health are not well understood. In the course of inflammatory processes, the Toll-like receptor 4 (TLR4) can sense damage-associated molecular patterns (DAMPs). Here, we investigate how the TLR4 response and pro-inflammatory potential of the proteinous DAMPs α-Synuclein (α-Syn), heat shock protein 60 (HSP60), and high-mobility-group box 1 protein (HMGB1), which are relevant in neurodegenerative and cardiovascular diseases, changes upon chemical modification with peroxynitrite.
For the peroxynitrite-modified proteins, we found a strongly enhanced activation of TLR4 and the pro-inflammatory transcription factor NF-κB in stable reporter cell lines as well as increased mRNA expression and secretion of the pro-inflammatory cytokines TNF-α, IL-1β, and IL-8 in human monocytes (THP-1). This enhanced activation of innate immunity via TLR4 is mediated by covalent chemical modifications of the studied DAMPs.
Our results show that proteinous DAMPs modified by peroxynitrite more potently amplify inflammation via TLR4 activation than the native DAMPs, and provide first evidence that such modifications can directly enhance innate immune responses via a defined receptor. These findings suggest that environmental pollutants and related ROS/RNS may play a role in promoting acute and chronic inflammatory disorders by structurally modifying the body's own DAMPs. This may have important consequences for chronic neurodegenerative, cardiovascular or gastrointestinal diseases that are prevalent in modern societies, and calls for action, to improve air quality and climate in the Anthropocene.
KW - Protein nitration
KW - Protein oligomerization
KW - Damage-associated molecular patterns (DAMPs)
KW - Pattern recognition receptor
KW - Anthropocene
KW - Environmental pollutants
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517128
DO - https://doi.org/10.1016/j.redox.2020.101581
VL - 37
SP - 101581
PB - Elsevier B.V.
AN - OPUS4-51712
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Brangsch, J.
A1 - Reimann, C.
A1 - Kaufmann, Jan Ole
A1 - Adams, L. C.
A1 - Onthank, D.
A1 - Thöne-Reineke, C.
A1 - Robinson, S.
A1 - Ponader, Marco
A1 - Weller, Michael G.
A1 - Buchholz, R.
A1 - Karst, U.
A1 - Botnar, R.
A1 - Hamm, B.
A1 - Makowski, M. R.
T1 - Molecular MR-Imaging for Noninvasive Quantification of the Anti-Inflammatory Effect of Targeting Interleukin-1β in a Mouse Model of Aortic Aneurysm
N2 - Background:
Molecular-MRI is a promising imaging modality for the assessment of abdominal aortic aneurysms (AAAs). Interleukin-1β (IL-1β) represents a new therapeutic tool for AAA-treatment, since pro-inflammatory cytokines are key-mediators of inflammation. This study investigates the potential of molecular-MRI to evaluate therapeutic effects of an anti-IL-1β-therapy on AAA-formation in a mouse-model.
Methods:
Osmotic-minipumps were implanted in apolipoprotein-deficient-mice (N = 27). One group (Ang-II+01BSUR group, n = 9) was infused with angiotensin-II (Ang-II) for 4 weeks and received an anti-murine IL-1β-antibody (01BSUR) 3 times. One group (Ang-II-group, n = 9) was infused with Ang-II for 4 weeks but received no treatment. Control-group (n = 9) was infused with saline and received no treatment. MR-imaging was performed using an elastin-specific gadolinium-based-probe (0.2 mmol/kg).
Results:
Mice of the Ang-II+01BSUR-group showed a lower aortic-diameter compared to mice of the Ang-II-group and control mice (p < 0.05). Using the elastin-specific-probe, a significant decrease in elastin-destruction was observed in mice of the Ang-II+01BSUR-group. In vivo MR-measurements correlated well with histopathology (y = 0.34x-13.81, R2 = 0.84, p < 0.05), ICP-MS (y = 0.02x+2.39; R2 = 0.81, p < 0.05) and LA-ICP-MS. Immunofluorescence and western-blotting confirmed a reduced IL-1β-expression.
Conclusions:
Molecular-MRI enables the early visualization and quantification of the anti-inflammatory-effects of an IL-1β-inhibitor in a mouse-model of AAAs. Responders and non-responders could be identified early after the initiation of the therapy using molecular-MRI.
KW - Cardiovascular
KW - Molecular-MRI
KW - Magnetic resonance imaging
KW - Gadolinium-based contrast agent
KW - Elastin-specific contrast agent ESMA
KW - Gadovist
KW - Gadofosveset
KW - MR Angiography
KW - Inductively Coupled Mass Spectroscopy
KW - Element Specific Bioimaging Using Laser Ablation
KW - Visualization
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517150
DO - https://doi.org/10.1177/1536012120961875
N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M.
VL - 19
SP - 61875
PB - SAGE
AN - OPUS4-51715
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Climent Terol, Estela
A1 - Biyikal, Mustafa
A1 - Gröninger, Delia
A1 - Weller, Michael G.
A1 - Martínez Mánez, R.
A1 - Rurack, Knut
ED - Climent Terol, Estela
T1 - Multiplexed Detection of Analytes on Single Test Strips with Antibody-Gated Indicator-Releasing Mesoporous Nanoparticles
N2 - Rapid testing methods for the use directly at apointof need are expected to unfold their true potential especiallywhen offering adequate capabilities for the simultaneousmeasurement of multiple analytes of interest. Considering theunique modularity,high sensitivity,and selectivity of antibody-gated indicator delivery (gAID) systems,amultiplexed assayfor three small-molecule explosives (TATP, TNT,PETN) wasthus developed, allowing to detect the analytes simultaneouslywith asingle test strip at lower ppb concentrations in the liquidphase in < 5min using afluorescence reader or asmartphonefor readout. While the TNT and PETN systems were newlydeveloped here,all the three systems also tolerated harshermatrices than buffered aqueous model solutions.Besidesasingle-track strip,the outstanding modularity of the hybridbiosensor materials in combination with strip-patterningtechnologies allowed us to obtain amultichannel strip inastraightforwardmanner,offering comparable analyticalperformance while allowing to be tailored even more to theusersneed.
KW - Multiplexing
KW - Explosives detection
KW - Gated materials
KW - Fluorescence
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518424
DO - https://doi.org/10.1002/anie.202009000
SN - 1433-7851
SN - 1521-3773
VL - 59
IS - 52
SP - 23862
EP - 23869
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-51842
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Weller, Michael G.
T1 - The Protocol Gap
N2 - Although peer review is considered one of the main pillars of modern science, experimental methods and protocols seem to be not a rigorous subject of this process in many papers. Commercial equipment, test kits, labeling kits, previously published concepts, and standard protocols are often considered to be not worth a detailed description or validation. Even more disturbing is the extremely biased citation behavior in this context, which sometimes leads to surrogate citations to avoid low-impact journals, preprints, or to indicate traditional practices. This article describes some of these surprising habits and suggests some measures to avoid the most unpleasant effects, which in the long term may undermine the credibility of science as a whole.
KW - Validation
KW - Peer review
KW - Experiment
KW - Documentation
KW - Scientific publication
KW - Reproducibility crisis
KW - Replication crisis
KW - Trust
KW - Citation
KW - References
KW - Surrogate citations
KW - Impact
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521440
DO - https://doi.org/10.3390/mps4010012
SN - 2409-9279
VL - 4
IS - 1
SP - 1
EP - 5
PB - MDPI
CY - Basel
AN - OPUS4-52144
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Paul, Sagar
A1 - Dolai, Malay
A1 - Nanda Goswami, Juli
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Drew, Michael G. B.
A1 - Chattopadhyay, Shouvik
A1 - Sarkar, Rabi Sankar
A1 - Sunil, Appu
A1 - Novitchi, Ghenadie
A1 - Moreno-Pineda, Eufemio
A1 - Wernsdorfer, Wolfgang
T1 - From strong to weak interaction: Reconciling SQUID and μSQUID-EPR data in anomalous Co(ii) dimers
N2 - Magnetic molecules have been proposed as scaffolds for novel quantum technologies, ranging from quantum sensing and quantum memory to multilevel quantum bits (qudits) and fault-tolerant quantum computation. Integration of magnetic molecules into cutting-edge applications hinges on a deep understanding and tunability of their spin states. To date, the strategic manipulation of the local environment of the ion and careful selection of the magnetic core have enabled the desired tunability and scalability of the spin states. For such goals, however, extracting the anisotropic parameters that dictate the characteristics of the Spin Hamiltonian is challenging, especially for molecules consisting of multiple magnetic cores. We address these challenges by studying two cobalt(II) dinuclear systems, complicated by inherent spin–orbit coupling. We explore the magnetic properties of these systems in two temperature regimes: (i) at sub-Kelvin temperatures employing single crystals at 30 mK using a unique μSQUID-EPR technique that examines the microwave absorption peaks in the magnetisation data and their variation with field angle and frequency; and (ii) in bulk employing convectional SQUID magnetometry above 2 K i.e., χMT(T) and M(H). Unexpectedly, sub-Kelvin temperature investigations reveal a negligible interaction, whereas the SQUID data reveal a much stronger interaction between the Co(II) ions. An understanding of these data is developed based on a strong coupling model and the coupling of two moieties with a spin-effective ground state.
KW - cOBALT(II)-complex
KW - In situ complex formation
KW - Magnetic property
KW - Crystal structure
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641421
DO - https://doi.org/10.1039/D5QI01387A
SN - 2052-1553
SP - 1
EP - 13
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64142
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mishra, Rajesh K.
A1 - Minussi, F.B.
A1 - Kumari, Priyanka
A1 - Shahi, Rohit R.
A1 - Yadav, R.P.
A1 - Emmerling, Franziska
A1 - Araújo, E.B.
T1 - Effect of sintering temperature on structural, microstructural, and dielectric properties of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 multi-cations high entropy oxides
N2 - The study reports the effect of sintering temperature on structural, microstructural, and dielectric properties of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 spinel high-entropy oxides (HEOs) synthesized through the solid-state mechanochemistry method. The sintering of the ceramic powders was accomplished at three different temperatures (1000 ◦C, 1100 ◦C, and 1250 ◦C), followed by air quenching. XRD analysis along with Le-Bail refinement confirms that 1100 ◦C and 1250 ◦C sintered oxides comprised of a single cubic spinel phase (Fd3m), while 1000 ◦C sintered oxide contains constituent oxides and a spinel phase. The phase formation of oxides sintered at 1100 ◦C and 1250 ◦C has also been confirmed by Raman spectroscopic analysis. Microstructural analysis revealed that the aggregated particle size increases with the rise in sintering temperature. With the change in sintering temperature, the dielectric behavior of the ceramic changed extensively. The 1100 ◦C sintered ceramic exhibits high frequency-dependent behavior, whereas the 1250 ◦C sintered ceramic yields low frequency-dependent behavior. The 1250 ◦C sintered HEO exhibits low-loss tangent (tan δ = 0.01) with higher dielectric permittivity (εʹ = 44) at high frequency (1 MHz) compared to the 1100 ◦C sintered ceramic and many other conventional dielectrics.
Fractal concept and impedance analysis have been employed to correlate the microstructure-dielectric property relation of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 spinel HEOs. The found Hurst exponent values for both different temperature-sintered HEOs are less than 0.5, indicating the anti-persistent behavior. This signifies that the height variations at neighboring pixels are negatively correlated. The present work is of fundamental importance in employing fractal analysis for the first time on spinel HEOs and correlating their properties. It also shows that processing conditions can effectively tailor the dielectric properties of the materials.
KW - Multi-cations high entropy oxide
KW - Mechanochemistry
KW - Spinel structure
KW - Fractal and impedance spectroscopic analysis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647584
DO - https://doi.org/10.1016/j.ceramint.2025.09.256
SN - 0272-8842
VL - 51
IS - 27
SP - 55341
EP - 55354
PB - Elsevier Ltd.
AN - OPUS4-64758
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -