TY - JOUR
A1 - Karafiludis, Stephanos
A1 - Standl, Jacob
A1 - Ryll, Tom W.
A1 - Schwab, Alexander
A1 - Prinz, Carsten
A1 - Wolf, Jakob B.
A1 - Kruschwitz, Sabine
A1 - Emmerling, Franziska
A1 - Völker, Christoph
A1 - Stawski, Tomasz M.
T1 - High-Entropy Phosphate Synthesis: Advancements through Automation and Sequential Learning Optimization
N2 - Transition metal phosphates (TMPs) are extensively explored for electrochemical and catalytical applications due to their structural versatility and chemical stability. Within this material class, novel high-entropy metal phosphates (HEMPs)─containing multiple transition metals combined into a single-phase structure─are particularly promising, as their compositional complexity can significantly enhance functional properties. However, the discovery of suitable HEMP compositions is hindered by the vast compositional design space and complex or very specific synthesis conditions. Here, we present a data-driven strategy combining automated wet-chemical synthesis with a Sequential Learning App for Materials Discovery (SLAMD) framework (Random Forest regression model) to efficiently explore and optimize HEMP compositions. Using a limited set of initial experiments, we identified multimetal compositions in a single-phase crystalline solid. The model successfully predicted a novel Co0.3Ni0.3Fe0.2Cd0.1Mn0.1 phosphate octahydrate phase, validated experimentally, demonstrating the effectiveness of the machine learning approach. This work highlights the potential of integrating automated synthesis platforms with data-driven algorithms to accelerate the discovery of high-entropy materials, offering an efficient design pathway to advanced functional materials.
KW - Metal phosphates
KW - High entropy
KW - Sequential learning
KW - Automated synthesis
KW - MAP
KW - Random forest
KW - Machine learning
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641554
DO - https://doi.org/10.1021/acs.cgd.5c00549
SN - 1528-7483
VL - 25
IS - 19
SP - 7989
EP - 8001
PB - American Chemical Society (ACS)
CY - Washington, DC
AN - OPUS4-64155
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Batteas, James
A1 - Blank, Kerstin G.
A1 - Colacino, Evelina
A1 - Emmerling, Franziska
A1 - Friščić, Tomislav
A1 - Mack, James
A1 - Moore, Jeffrey
A1 - Rivas, Maria Elena
A1 - Tysoe, Wilfred
T1 - Moving mechanochemistry forward
N2 - Arguably mechanochemistry is one of the oldest, and at the same time one of the newest, areas of chemistry. One of the oldest, because it has been theorized that early hominids were able to develop rapidly due to their ability to heat and mechanically process their food to make it easier to digest. Old, because the ancient Greeks knew that mechanically activating stones (consisting of cinnabar) with vinegar in a copper pestle and mortar caused them to convert into mercury. We might be forgiven for thinking that this could have led our alchemical forbears to wonder if there were other stones that might also be persuaded to convert into gold. Early chemical luminaries such as Michael Faraday and Wilhelm Röntgen dabbled in mechanochemistry. However, in the late 19th and early 20th centuries, the field developed separately in many areas. Perhaps most significantly, synthetic chemists realized that reactions could be carried out with surprisingly high yields and selectivities by shaking them in a ball mill, and that they could even make novel compounds that their colleagues just using heat were not able to. Physicists were mechanically rearranging atoms into new configurations (i.e., doing chemistry) using exotic means such as atomic force microscope tips and optical tweezers. Scientists and engineers studying the formation of lubricious and anti-wear films realized that they were mechanochemically formed. Biochemists found molecular motor proteins, such as myosin and kinesin, that were able to convert chemical energy into motion or, vice versa, mechanical energy into the biochemical energy storage molecule adenosine triphosphate. In 2023, this confluence of advances convinced the Royal Society of Chemistry that the time was ripe to establish a new journal dedicated to the field of mechanochemistry. It is rare that a journal has the privilege of helping to create a new sub-branch of chemistry but, having done so, it has the obligation of helping to define the field and, optimistically, suggesting how the field might develop. This editorial has two major goals. The first is to bring to the attention of the scientific community the challenges faced by the field to set people thinking about how they might contribute and, second, to form the basis for more thorough discussions in the future. The sub-topics below outline current thoughts brought forward from members of our editorial board. We lay out areas and topics here with the intent of establishing a new editorial series, which we invite the community to contribute to, and outline topics and hopefully lay out challenges, which will enable us as a community to come together to move mechanochemistry forward.
KW - Mechanochemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646086
DO - https://doi.org/10.1039/d4mr90021a
SN - 2976-8683
VL - 2
IS - 1
SP - 10
EP - 19
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64608
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ferreira, Daniela R.
A1 - Portet, Anaïs
A1 - Alves, Paula C.
A1 - Rijo, Patrícia
A1 - Gomes, Clara S. B.
A1 - Duarte, M. Teresa
A1 - Halasz, Ivan
A1 - Colacino, Evelina
A1 - Emmerling, Franziska
A1 - André, Vânia
T1 - Modulating the crystalline forms of silver–sulfadiazine complexes by mechanochemistry
N2 - Mechanochemical synthesis of pharmaceutical compounds has gained significant attention due to its potential to overcome traditional synthetic challenges while offering the possibility of improving the physicochemical properties of drugs. This study delves into the mechanochemical synthesis of silver sulfadiazine (AgSD) coordination compounds, obtained under different mechanochemical stress and processing conditions. The aim of this work was to investigate the influence of mechanochemical conditions on the selectivity in the preparation of AgSD coordination compounds. Through a series of experiments, we demonstrate the successful synthesis of two different AgSD coordination networks, using high-energy ball milling. By strategically manipulating the starting materials and milling parameters — including milling time, milling frequency, type of mechanical stress (as determined by different milling devices), and the presence of co-milling agents — we were able to control the product outcome. As a result, we achieved two different forms of silver-sulfadiazine metal frameworks, one of which was not previously disclosed. The crystal structure of the new form, obtained from high resolution PXRD synchrotron data, was compared with the previously known structure of a silver sulfadiazine compound. The in-depth antimicrobial activity systematic study of these AgSD forms on the generic systems showed increased antibacterial activity when compared to sulfadiazine. This research sheds light on the mechanochemical synthesis of silver sulfadiazine complexes. The obtained knowledge may guide the development of novel synthetic strategies for other drug molecules, leading to improved drug performance, stability, and therapeutic outcomes.
KW - Mechanochemistry
KW - Structure solution
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646099
DO - https://doi.org/10.1039/d5ce00572h
SN - 1466-8033
SP - 1
EP - 12
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64609
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez-Sánchez, Noelia
A1 - Prinz, Carsten
A1 - Bienert, Ralf
A1 - Ballesteros, Menta
A1 - Ruiz Salvador, A. Rabdel
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Mechanochemical ZIF-9 formation: in situ analysis and photocatalytic enhancement evaluation
N2 - Efficient treatment of persistent pollutants in wastewater is crucial for sustainable water management and environmental protection. This study addresses this challenge by investigating the mechanochemical synthesis and photocatalytic performance of ZIF-9, a cobalt-based zeolitic imidazolate framework. Using synchrotron-based powder X-ray diffraction, we provide real-time insights into the formation dynamics of ZIF-9 during mechanosynthesis. Our results show that mechanochemically synthesised ZIF-9 exhibits superior photocatalytic activity compared to its solvothermally prepared counterpart, achieving a 2-fold increase in methylene blue degradation rate. This research not only advances our understanding of the synthesis and properties of ZIF-9, but also demonstrates the potential of mechanochemical approaches in the development of high-performance, sustainably produced materials for water treatment and other environmental applications.
KW - MOFs
KW - ZIF
KW - Time-resolved in situ investigation
KW - Photocatalysis synchrotron X-ray powder diffraction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641416
DO - https://doi.org/10.1039/D4MR00114A
SN - 2976-8683
VL - 2
IS - 1
SP - 116
EP - 126
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64141
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lopes, Chrystal
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Leyssens, Tom
A1 - Dupray, Valérie
A1 - Brandel, Clement
A1 - Cartigny, Yohann
T1 - Efficient racemization of the pharmaceutical compound Levetiracetam using solvent-free mechanochemistry
N2 - We present the racemization of an active pharmaceutical ingredient Levetiracetam using a novel approach. We demonstrate the design of a 100% solvent-free process that proceeds by high energy milling inside a regular mixer mill. The kinetics of the racemization process is drastically improved compared to the solution-based approach and illustrates the tremendous potential of mechanochemistry. In this study, we highlight the importance of mixing efficiency regarding data reproducibility, and we show, in particular, that water contamination has a negative impact on the reaction rate. Moreover, in situ X-ray diffraction gives us first insights into the mechanisms involved in the solid state during the mechanochemical racemization process.
KW - Mechanochemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646108
DO - https://doi.org/10.1039/d4mr00103f
SN - 2976-8683
VL - 2
IS - 1
SP - 83
EP - 90
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64610
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Macchietti, Laura
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Braga, Dario
A1 - Grepioni, Fabrizia
T1 - Deriving kinetic insights from mechanochemically synthesized compounds using multivariate analysis (MCR-ALS) of powder X-ray diffraction data
N2 - Kinetics information on the progress of the mechanochemical reactions is key to their understanding and subsequent scale-up. For crystalline materials, the most robust and tested method for obtaining kinetic data is the Quantitative Phase Analysis (QPA) via Rietveld refinement. In this work, we tested the feasibility of the Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS) method on powder X-ray diffraction (PXRD) data of mechanochemical processes by studying the system theophylline (TP) and malonic acid (MA) in a 1 : 1 stoichiometric ratio at different milling conditions. We have highlighted the strengths and weaknesses of the MCR-ALS method, and we demonstrated why it may be an alternative route to obtain quantitative information on mechanochemical kinetics.
KW - Mechanochemistry
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646115
DO - https://doi.org/10.1039/d3mr00013c
SN - 2976-8683
VL - 1
IS - 1
SP - 106
EP - 115
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64611
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pavlidis, Sotirios
A1 - Teutloff, Christian
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Krause, Konstantin B.
A1 - Emmerling, Franziska
A1 - Bittl, Robert
A1 - Abbenseth, Josh
T1 - A Crystalline Bismuth(II) Radical Anion: Synthesis, Characterization, and Reactivity
N2 - AbstractWe report the synthesis of a planarized tris‐amidobismuthane supported by a rigid, bulky NNN pincer ligand, which enforces a T‐shaped geometry at the bismuth center. The Bi(NNN) complex features a low‐lying LUMO with distinct Bi(6p) orbital character as shown by DFT calculations. Cyclic voltammetry reveals a fully reversible one‐electron reduction at E1/2 = –1.85 V versus Fc0/+ in THF. Chemical reduction with KC8 in the presence of 4,7,13,16,21,24‐hexaoxa‐1,10‐diazabicyclo[8.8.8]hexacosane (222‐crypt) enables the isolation of an unprecedented Bi(II) radical anion in high isolated yields. Multi‐frequency EPR, X‐ray absorption spectroscopy and SQUID magnetometry complemented by theoretical calculations confirm localization of the unpaired electron on the bismuth center. Preliminary reactivity studies display radical reactivity as shown by single‐electron transfer chemistry and radical coupling reactions.
KW - Bi(III)
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644143
DO - https://doi.org/10.1002/anie.202515545
SN - 1433-7851
VL - 64
IS - 49
SP - 1
EP - 6
PB - Wiley VHC-Verlag
AN - OPUS4-64414
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Chapartegui-Arias, Ander
A1 - Raysyan, A.
A1 - Belenguer, A. M.
A1 - Jaeger, Carsten
A1 - Tchipilov, Teodor
A1 - Prinz, Carsten
A1 - Abad Andrade, Carlos Enrique
A1 - Beyer, S.
A1 - Schneider, Rudolf
A1 - Emmerling, Franziska
T1 - Tailored mobility in a zeolite imidazolate framework (ZIF) antibody conjugate
N2 - Zeolitic imidazolate framework (ZIF) hybrid fluorescent nanoparticles and ZIF antibody conjugates have been synthesized, characterized, and employed in lateral-flow immunoassay (LFIA). The bright fluorescence of the conjugates and the possibility to tailor their mobility gives a huge potential for diagnostic assays. An enzyme-linked immunosorbent assay (ELISA) with horseradish peroxidase (HRP) as label, proved the integrity, stability, and dispersibility of the antibody conjugates, LC-MS/MS provided evidence that a covalent link was established between these metal-organic frameworks and lysine residues in IgG antibodies.
KW - ZIF
KW - ELISA
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532096
DO - https://doi.org/10.1002/chem.202100803
SN - 0947-6539
SN - 1521-3765
VL - 27
IS - 36
SP - 9414
EP - 9421
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-53209
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Casali, L.
A1 - Broll, V.
A1 - Ciurili, S.
A1 - Braga, D.
A1 - Emmerling, Franziska
A1 - Gepioni, F.
T1 - Facilitating Nitrification Inhibition through Green, Mechanochemical Synthesis of a Novel Nitrapyrin Complex
N2 - Nitrapyrin (NP) is applied to cultivated soils to inhibit the enzymatic activity of ammonia monooxygenase (AMO), but its poor aqueous solubility and high volatility severely limit its application. β-Cyclodextrin (β-CD) is commonly used to form inclusion complexes with hydrophobic molecules, improving water solubility and stability upon complexation. Here we report on the mechanochemical synthesis of the inclusion complex β-CD·NP, characterized via a combination of solid-state techniques, including exsitu and in situ X-ray diffraction, Raman and NMR spectroscopies, transmission electron microscopy, and energy dispersive X-ray spectroscopy. The pure inhibitor NP was also structurally characterized. The β-CD·NP complex presents improved solubility and thermal stability, and still inhibits the enzymatic activity of AMO with high efficacy. All results indicate that the inclusion of NP into β-CD represents a viable route for the preparation of a novel class of inhibitors, with improved properties related to stability, water solubility, and good inhibition activity.
KW - Mechanochemistry
KW - Nitrification
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537154
DO - https://doi.org/10.1021/acs.cgd.1c00681
SN - 1528-7505
VL - 21
IS - 10
SP - 5792
EP - 5799
PB - ACS Publications
AN - OPUS4-53715
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heilmann, Maria
A1 - Prinz, Carsten
A1 - Bienert, Ralf
A1 - Wendt, R.
A1 - Kunkel, B.
A1 - Radnik, Jörg
A1 - Hoell, A.
A1 - Wohlrab, S.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Emmerling, Franziska
T1 - Size-Tunable Ni–Cu Core–Shell Nanoparticles—Structure, Composition, and Catalytic Activity for the Reverse Water–Gas Shift Reaction
N2 - A facile and efficient methodology is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core–shell nanoparticles (NPs) for application in catalysis. The diameter of the NPs is tuned in a range from 6 nm to 30 nm and to adjust the Ni:Cu ratio from 30:1 to 1:1. Furthermore, the influence of different reaction parameters on the final NPs is studied. The NPs are structurally characterized by a method combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray absorption fine structure, and X-ray photoelectron spectroscopy. Using these analytical methods, it is possible to elucidate a core–shell–shell structure of all particles and their chemical composition. In all cases, a depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core–shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction) independent of size and Ni:Cu ratio.
KW - Nanoparticles
KW - Core-shell
KW - Catalysis
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543606
DO - https://doi.org/10.1002/adem.202101308
SN - 1438-1656
SP - 1
EP - 13
PB - Wiley VCH
AN - OPUS4-54360
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dudziak, Mateusz
A1 - Topolniak, Ievgeniia
A1 - Silbernagl, Dorothee
A1 - Altmann, Korinna
A1 - Sturm, Heinz
T1 - Long-time behavior of surface properties of microstructures fabricated by multiphoton lithography
N2 - The multiphoton lithography (MPL) technique represents the future of 3D microprinting, enabling the production of complex microscale objects with high precision. Although the MPL fabrication parameters are widely evaluated and discussed, not much attention has been given to the microscopic properties of 3D objects with respect to their surface properties and time-dependent stability. These properties are of crucial importance when it comes to the safe and durable use of these structures in biomedical applications. In this work, we investigate the surface properties of the MPL-produced SZ2080 polymeric microstructures with regard to the physical aging processes during the post-production stage. The influence of aging on the polymeric microstructures was investigated by means of Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS). As a result, a time-dependent change in Young’s Modulus, plastic deformation, and adhesion and their correlation to the development in chemical composition of the surface of MPL-microstructures are evaluated. The results presented here are valuable for the application of MPL-fabricated 3D objects in general, but especially in medical technology as they give detailed information of the physical and chemical time-dependent dynamic behavior of MPL-printed surfaces and thus their suitability and performance in biological systems.
KW - Multiphoton lithography
KW - Additive manufacturing
KW - Microfabrication
KW - SZ2080 negative photo-resist
KW - Young´s modulus
KW - Aging
KW - Surface properties
KW - X-ray photoelectron spectroscopy
KW - Atomic force microscopy
KW - Force-distance-curve
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542166
DO - https://doi.org/10.3390/nano11123285
SN - 2079-4991
VL - 11
IS - 12
SP - 1
EP - 12
PB - MDPI
CY - Basel
AN - OPUS4-54216
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Müller, Axel
A1 - Altmann, Korinna
A1 - Kocher, B.
A1 - Braun, U.
T1 - Determination of tire wear markers in soil samples and their distribution in a roadside soil
N2 - Tire wear (TW) constitutes a significant source of microplastic in terrestrial ecosystems. It is known that particles emitted by roads can have an effect up to 100 m into adjacent areas. Here, we apply for the first-time thermal extraction desorption gas chromatography-mass spectrometry (TED-GC/MS) to determine TW in soil samples by detection of thermal decomposition products of styrene-butadiene rubber (SBR), without additional enrichment. Additionally, zinc contents were determined as an elemental marker for TW. Mixed soil samples were taken along three transects along a German motorway in 0.3, 2.0, and 5.0 m distance from the road. Sampling depths were 0–2, 2–5, 5–10, and 10–20 cm. Four fine fractions, 1 000–500, 500–100, 100–50, and <50 μm, were analyzed.
TW contents based on SBR ranged from 155 to 15 898 mg kg−1. TW contents based on zinc were between 413 and 44 812 mg kg−1. Comparison of individual values of SBR and zinc reveals SBR as a more specific marker. Results confirm that most TW ends up in the topsoil within a 2 m distance.
The sampling strategy resulted in representative data for a larger area. Standard deviations of quadruple TED-GC/MS determination of SBR were <10% for all grain size fractions. TED-GC/MS is a suitable analytical tool for determining TW in soil samples without the use of toxic chemicals, enrichment, or special sample preparation.
KW - Microplastic
KW - TED-GC/MS
KW - Tire wear
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543344
DO - https://doi.org/10.1016/j.chemosphere.2022.133653
VL - 294
SP - 1
EP - 8
PB - Elsevier Ltd.
AN - OPUS4-54334
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Yusenko, Kirill
A1 - Kabelitz, Anke
A1 - Schokel, Alexander
A1 - Wagner, Ralf
A1 - Prinz, Carsten
A1 - Kemnitz, E
A1 - Emmerling, Franziska
A1 - Krahl, Thoralf
A1 - de Oliveira Guilherme Buzanich, Ana
T1 - Local Structure of Europium-Doped Luminescent Strontium Fluoride Nanoparticles: Comparative X-ray Absorption Spectroscopy and Diffraction Study
N2 - Rare-earth based luminescent materials are key functional components for the rational design of light-conversion smart devices. Stable Eu3+-doped strontium fluoride (SrF2) nanoparticles were prepared at room temperature in ethylene glycol. Their luminescence depends on the Eu content and changes after heat treatment. The crystallinity of heat-treated material increases in comparison with as-synthesized samples. Particles were investigated in solution using X-ray diffraction, small-angle X-ray scattering, and X-ray spectroscopy. After heat treatment, the size of the disordered nanoparticles increases together with a change of their local structure. Interstitial fluoride ions can be localized near Eu3+ ions. Therefore, non-radiative relaxation from other mechanisms is decreased. Knowledge about the cation distribution is key information for understanding the luminescence properties of any material.
KW - SrF2
KW - EXAFS
KW - Eu
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540094
DO - https://doi.org/10.1002/cnma.202100281
VL - 7
IS - 11
SP - 1221
EP - 1229
PB - Wiley Online Library
AN - OPUS4-54009
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lampronti, G.
A1 - Michalchuk, Adam
A1 - Mazzeo, P.
A1 - Belenguer, Ana
A1 - Sanders, J. K. M.
A1 - Bacchi, A.
A1 - Emmerling, Franziska
T1 - Changing the game of time resolved X-ray diffraction on the mechanochemistry playground by downsizing
N2 - Time resolved in situ (TRIS) monitoring has revolutionised the study of mechanochemical transformations but has been limited by available data quality. Here we report how a combination of miniaturised grinding jars together with innovations in X-ray powder diffraction data collection and state-of-the-art analysis strategies transform the power of TRIS synchrotron mechanochemical experiments. Accurate phase compositions, comparable to those obtained by ex situ measurements, can be obtained with small sample loadings. Moreover, microstructural parameters (crystal size and microstrain) can be also determined with high confidence. This strategy applies to all chemistries, is readily implemented, and yields high-quality diffraction data even using a low energy synchrotron source. This offers a direct avenue towards the mechanochemical investigation of reactions comprising scarce, expensive, or toxic compounds. Our strategy is applied to model systems, including inorganic, metal-organic, and organic mechanosyntheses, resolves previously misinterpreted mechanisms in mechanochemical syntheses, and promises broad, new directions for mechanochemical research.
KW - Mechanochemistry
KW - Synchrotron radiation
KW - Material synthesis
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535932
DO - https://doi.org/10.1038/s41467-021-26264-1
SN - 2041-1723
VL - 12
IS - 1
SP - 1
EP - 9
PB - Nature Publishing Group
CY - London
AN - OPUS4-53593
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Feiler, Torvid
A1 - Michalchuk, Adam
A1 - Schröder, V.
A1 - List-Kratochvil, E.
A1 - Emmerling, Franziska
A1 - Bhattacharya, Biswajit
T1 - Elastic Flexibility in an Optically Active Naphthalidenimine-Based Single Crystal
N2 - Organic single crystals that combine mechanical flexibility and optical properties are important for developing flexible optical devices, but examples of such crystals remain scarce. Both mechanical flexibility and optical activity depend on the underlying crystal packing and the nature of the intermolecular interactions present in the solid state. Hence, both properties can be expected to be tunable by small chemical modifications to the organic molecule. By incorporating a chlorine atom, a reportedly mechanically flexible crystal of (E)-1-(4-bromo-phenyl)iminomethyl-2-hydroxylnaphthalene (BPIN) produces (E)-1-(4-bromo-2-chloro-phenyl)iminomethyl-2-hydroxyl-naphthalene (BCPIN). BCPIN crystals show elastic bending similar to BPIN upon mechanical stress, but exhibit a remarkable difference in their optical properties as a result of the chemical modification to the backbone of the organic molecule. This work thus demonstrates that the optical properties and mechanical flexibility of molecular materials can, in principle, be tuned independently.
KW - Elastic Crystal
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539040
DO - https://doi.org/10.3390/cryst11111397
VL - 11
IS - 11
SP - 1397
PB - MDPI
AN - OPUS4-53904
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gernhard, M.
A1 - Rautenberg, Max
A1 - Hörner, G.
A1 - Weber, B.
A1 - Emmerling, Franziska
A1 - Roth, C.
T1 - Mechanochemical Synthesis as a Greener Way to ProduceIron-based Oxygen Reduction Catalysts
N2 - Iron-based catalysts have been reported manifold and studied as platinum group metal (PGM) free alternatives for the catalysis of the oxygen reduction reaction (ORR). However, their sustainable preparation by greener synthesis approaches is usually not discussed. In this work, we propose a new method for the sustainable preparation of such catalysts by using a mechanochemical approach, with no solvents and non-toxic chemicals. The materials obtained from low temperature carbonization (700 °C) exhibit considerable and stable catalytic performance for ORR in alkaline medium. A catalyst obtained
from iron hydroxide, tryptophan, dicyandiamide, and ammonium nitrate shows the best electrocatalytic Performance with an overpotential of 921 mV vs. RHE at 0.1 mA/cm2 and an electron transfer number of 3.4.
KW - PGM-free catalyst
KW - Oxygen Reduction Reaction
KW - AEMFC
KW - Mössbauer Spectroscopy
KW - Sustainable Synthesis
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535326
DO - https://doi.org/10.1002/zaac.202100194
VL - 647
IS - 22
SP - 2080
EP - 2087
PB - Weinheim-VCH GmbH
AN - OPUS4-53532
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Michalchuk, Adam
A1 - Rudic, S.
A1 - Pulham, C.
A1 - Morrison, C.
T1 - Predicting the impact sensitivity of a polymorphic high explosive: the curious case of FOX-7
N2 - The impact sensitivity (IS) of FOX-7 polymorphs is predicted by phonon up-pumping to decrease as layers of FOX-7 molecules flatten. Experimental validation proved anomalous owing to a phase transition during testing, raising questions regarding Impact sensitivity measurement and highlighting the need for models to predict IS of polymorphic energetic materials.
KW - Energetic materials
KW - Density functional theory
KW - Inelastic Neutron Scattering Spectroscopy
KW - Impact Sensitivity
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535558
DO - https://doi.org/10.1039/d1cc03906g
SN - 1364-548X
VL - 57
IS - 85
SP - 11213
EP - 11216
PB - Royal Society of Chemistry
AN - OPUS4-53555
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Loges, A.
A1 - Scholz, G.
A1 - de Sousa Amadeu, Nader
A1 - Jingjing, S.
A1 - Emmerling, Franziska
A1 - John, T.
A1 - Paulus, B.
A1 - Braun, T.
T1 - Studies on the local structure of the F/OH site in topaz by magic angle spinning nuclear magnetic resonance and Raman spectroscopy
N2 - he mutual influence of F and OH groups in neighboring sites in topaz (Al2SiO4(F,OH)2) was investigated using magic angle spinning nuclear magnetic resonance (MAS NMR) and Raman spectroscopy. The splitting of 19F and 1H NMR signals, as well as the OH Raman band, provides evidence for hydrogen bond formation within the crystal structure. Depending on whether a given OH group has another OH group or fluoride as its neighbor, two different hydrogen bond constellations may form: either OH···O···HO or F···H···O. The proton accepting oxygen was determined to be part of the SiO4 tetrahedron using 29Si MAS NMR. Comparison of the MAS NMR data between an OH-bearing and an OH-free topaz sample confirms that the 19F signal at −130 ppm stems from F− ions that take part in H···F bonds with a distance of ∼ 2.4 Å, whereas the main signal at −135 ppm belongs to fluoride ions with no immediate OH group neighbors. The Raman OH sub-band at 3644 cm−1 stems from OH groups neighboring other OH groups, whereas the sub-band at 3650 cm−1 stems from OH groups with fluoride neighbors, which are affected by H···F bridging. The integrated intensities of these two sub-bands do not conform to the expected ratios based on probabilistic calculations from the total OH concentration. This can be explained by a difference in the polarizability of the OH bond between the different hydrogen bond constellations or partial order or unmixing of F and OH, or a combination of both. This has implications for the quantitative interpretation of Raman data on OH bonds in general and their potential use as a probe for structural (dis-)order. No indication of tetrahedrally coordinated Al was found with 27Al MAS NMR, suggesting that the investigated samples likely have nearly ideal Al/Si ratios, making them potentially useful as high-density electron microprobe reference materials for Al and Si, as well as for F.
KW - Topas
KW - NMR
KW - XRD
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561863
DO - https://doi.org/10.5194/ejm-34-507-2022
SN - 1617-4011
VL - 34
IS - 5
SP - 507
EP - 521
PB - Copernicus Publications
CY - Göttingen
AN - OPUS4-56186
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mazzeo, P. P.
A1 - Prencipe, M.
A1 - Feiler, Torvid
A1 - Emmerling, Franziska
A1 - Bacchi, A.
T1 - On the mechanism of cocrystal mechanochemical reaction via low melting eutectic: A time-resolved in situ monitoring investigation
N2 - Mechanochemistry has become a sustainable and attractive cost-effective synthetic technique, largely used within the frame of crystal engineering. Cocrystals, namely, crystalline compounds made of different chemical entities within the same crystal structure, are typically synthesized in bulk via mechanochemistry; however, whereas the macroscopic aspects of grinding are becoming clear, the fundamental principles that underlie mechanochemical cocrystallization at the microscopic level remain poorly understood. Time-resolved in situ (TRIS) monitoring approaches have opened the door to exceptional detail regarding mechanochemical reactions. We here report a clear example of cocrystallization between two solid coformers that proceeds through the formation of a metastable low melting binary eutectic phase. The overall cocrystallization process has been monitored by time-resolved in situ (TRIS) synchrotron X-ray powder diffraction with a customized ball milling setup, currently available at μ Spot beamline at BESSY-II, Helmholtz-Zentrum Berlin. The binary system and the low melting eutectic phase were further characterized via DSC, HSM, and VT-XRPD.
KW - Mechanochemistry
KW - In situ
KW - Cocrystal
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552977
DO - https://doi.org/10.1021/acs.cgd.2c00262
SN - 1528-7505
VL - 22
IS - 7
SP - 4260
EP - 4267
PB - ACS Publ.
CY - Washington, DC
AN - OPUS4-55297
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pakrashy, S.
A1 - Mandal, P. K.
A1 - Goswami, J. N.
A1 - Dey, S. K.
A1 - Choudhury, S. M.
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Alasmary, F. A.
A1 - Dolai, M.
T1 - Bioinformatics and Network Pharmacology of the First Crystal Structured Clerodin: Anticancer and Antioxidant Potential against Human Breast Carcinoma Cell
N2 - Clerodin was isolated from the medicinal plant Clerodendrum infortunatum, and CSD search showed the first crystal structure of clerodin by a single-crystal X-ray diffraction study. We checked its binding potential with target proteins by docking and conducted network pharmacology analysis, ADMET analysis, in silico pathway analysis, normal mode analysis (NMA), and cytotoxic activity studies to evaluate clerodin as a potential anticancer agent. The cell viability studies of clerodin on the human breast carcinoma cell line (MCF-7) showed toxicity on MCF-7 cells but no toxicity toward normal human lymphocyte cells (HLCs). The anticancer mechanism of clerodin was validated by its enhanced capacity to produce intracellular reactive oxygen species (ROS) and to lower the reduced glutathione content in MCF-7 cells.
KW - Anticancer
KW - Clerodin
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567600
DO - https://doi.org/10.1021/acsomega.2c07173
SN - 2470-1343
VL - 7
IS - 51
SP - 48572
EP - 48582
PB - ACS Publ.
CY - Washington, DC
AN - OPUS4-56760
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Abusafia, A.
A1 - Scheid, C.
A1 - Meurer, Maren
A1 - Altmann, Korinna
A1 - Dittmer, U.
A1 - Steinmetz, H.
T1 - Microplastic sampling strategies in urban drainage systems for quantification of urban emissions based on transport pathways
N2 - Tracking waterborne microplastic (MP) in urban areas is a challenging task because of the various sources and transport pathways involved. Since MP occurs in low concentrations in most wastewater and stormwater streams, large sample volumes need to be captured, prepared, and carefully analyzed. The recent research in urban areas focused mainly on MP emissions at wastewater treatment plants (WWTPs), as obvious entry points into receiving waters. However, important transport pathways under wet-weather conditions are yet not been investigated thoroughly. In addition, the lack of comprehensive and comparable sampling strategies complicated the attempts for a deeper understanding of occurrence and sources. The goal of this paper is to (i) introduce and describe sampling strategies for MP at different locations in a municipal catchment area under dry and wet-weather conditions, (ii) quantify MP emissions from the entire catchment and two other smaller ones within the bigger catchment, and (iii) compare the emissions under dry and wet-weather conditions. WWTP has a high removal rate of MP (>96%), with an estimated emission rate of 189 kg/a or 0.94 g/[population equivalents (PEQ · a)], and polyethylene (PE) as the most abundant MP. The specific dry-weather emissions at a subcatchment were ≈30 g/(PEQ · a) higher than in the influent of WWTP with 23 g/(PEQ · a). Specific wet-weather emissions from large sub-catchment with higher traffic and population densities were 1952 g/(ha · a) higher than the emissions from smaller catchment (796 g/[ha · a]) with less population and traffic. The results suggest that wet-weather transport pathways are likely responsible for 2–4 times more MP emissions into receiving waters compared to dry-weather ones due to tire abrasion entered from streets through gullies. However, more investigations of wet-weather MP need to be carried out considering additional catchment attributes and storm event characteristics.
KW - Combined sewer system
KW - Large volume samplers
KW - Microplastic pollution
KW - Separate sewer system
KW - Stormwater retention tank
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568271
DO - https://doi.org/10.1002/appl.202200056
SP - 1
EP - 12
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-56827
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rautenberg, Max
A1 - Bhattacharya, Biswajit
A1 - Witt, Julia
A1 - Jain, Mohit
A1 - Emmerling, Franziska
T1 - In situ time-resolved monitoring of mixed-ligand metal–organic framework mechanosynthesis
N2 - The mechanism of mixed-ligand metal–organic framework (MOF) formation, and the possible role of intermediate single-ligand metal complexes during mechanosynthesis, have not been explored yet. For the first time, we report here in situ real-time monitoring of the mechanochemical formation mechanism of mixed-ligand MOFs. Our results show that binary phases can act as intermediates or competing products in one-pot and stepwise synthesis.
KW - Mechanochemistry
KW - Metal-organic-frameworks
KW - In situ X-ray diffraction
KW - Mixed-ligand MOFs
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558167
DO - https://doi.org/10.1039/D2CE00803C
SP - 1
EP - 4
PB - Royal Society of Chemistry
AN - OPUS4-55816
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Emmerling, Franziska
A1 - Hoch, C.
T1 - Laudatio Prof. Dr.-Ing. Caroline Röhr
N2 - It is a laudatio on the ocations of Prof. Dr.-Ing. Caroline Röhrs 60th birthday.
KW - Metal-oxides
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561877
DO - https://doi.org/10.1002/zaac.202200159
SN - 0044-2313
VL - 648
IS - 10
SP - 1
EP - 2
PB - John Wiley & Sons, Ltd
AN - OPUS4-56187
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kadri, Lena
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Tajber, Lidia
T1 - Mechanochemical comparison of ball milling processes for levofloxacin amorphous polymeric systems
N2 - This study aimed to investigate the amorphization capabilities of levofloxacin hemihydrate (LVXh), a fluoroquinolone drug, using a polymer excipient, Eudragit® L100 (EL100). Ball milling (BMing) was chosen as the manufacturing process and multiple mill types were utilized for comparison purposes. The product outcomes of each mill were analyzed in detail. The solid-state of the samples produced was comprehensively characterized by Powder X-ray Diffraction (PXRD), In-situ PXRD, Differential Scanning Calorimetry (DSC), Solid-State Fourier Transform Infrared Spectroscopy (FT-IR), and Dynamic Vapor Sorption (DVS). The crystallographic planes of LVXh were investigated by in-situ PXRD to disclose the presence or absence of weak crystallographic plane(s). The mechanism of LVXh:EL100 system formation was discovered as a two-step process, first involving amorphization of LVXh followed by an interaction with EL100, rather than as an instantaneous process. DVS studies of LVXh:EL100 samples showed different stability properties depending on the mill used and % LVXh present. Overall, a more sustainable approach for achieving full amorphization of the fluoroquinolone drug, LVXh, was accomplished, and advancements to the fast-growing world of pharmaceutical mechano- and tribo-chemistry were made.
KW - Levofloxacin
KW - Eudragit® L100
KW - Mechanochemistry
KW - Phase transformation
KW - In situ monitoring
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611129
DO - https://doi.org/10.1016/j.ijpharm.2024.124652
SN - 0378-5173
VL - 665
SP - 1
EP - 16
PB - Elsevier B.V.
AN - OPUS4-61112
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Baláž, Matej
A1 - Birinci, Mustafa
A1 - Şentürk, Kader
A1 - Achimovičová, Marcela
A1 - Baláž, Peter
A1 - Tampubolon, Imelda Octa
A1 - Stolar, Tomislav
A1 - Bienert, Ralf
A1 - Emmerling, Franziska
A1 - Erdemoğlu, Sema
A1 - Sis, Hikmet
A1 - Erdemoğlu, Murat
T1 - Utilizing Taguchi method and in situ X-ray powder diffraction monitoring to determine the influence of mechanical activation conditions on the physico-chemical properties and Al leachability of K-feldspar
N2 - K-feldspar represents an important natural resource of potassium and aluminum. Within the framework of this study, the K-feldspar was mechanically activated in a planetary ball mill under different conditions planned according to 43 Taguchi orthogonal array experimental design. As outputs, specific surface area (SBET), median particle size (d50), amorphization degree of mineral phases , and Al recovery were used. It was found that the initial d50 value of 293 μm could be reduced to 6.7 μm and the SBET value of 4.7 m2/g could be increased up to 32.5 m2/g upon milling. Both microcline KAl3SiO8, and albite NaAl3SiO8 could be almost completely amorphized, whereas quartz SiO2 still maintained some crystallinity even under the most intensive conditions. Increasing SBET and decreasing the d50 values did not lead to a significant improvement in Al leach recovery, whereas a clear relationship between the amorphization of microcline and the recovered aluminum was found. Analysis of Variance (ANOVA) showed that increasing ball-to-powder ratio is the most beneficial for the improvement in Al recovery. In situ powder X-ray diffraction monitoring performed in an oscillation ball mill under synchrotron irradiation has shown very rapid amorphization of microcline phase at the beginning. However, amorphization of microcline was only partial after two hours of the treatment in this mill, apart from almost complete process in the planetary ball mill. In the end, regressions for the calculation of Al recovery by knowing the values of input parameters were calculated. In general, by just using mechanical activation without the subsequent roasting process that is commonly used to boost metal recoveries, it was possible to quantitatively recover aluminum from K-feldspar.
KW - Mechanochemistry
KW - Mechanical activation
KW - Design of experiments
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611059
DO - https://doi.org/10.1016/j.jmrt.2024.08.156
SN - 2238-7854
VL - 32
SP - 3886
EP - 3895
PB - Elsevier B.V.
AN - OPUS4-61105
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Cakir, Cafer Tufan
A1 - Bogoclu, Can
A1 - Emmerling, Franziska
A1 - Streli, Christina
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
T1 - Machine learning for efficient grazing-exit x-ray absorption near edge structure spectroscopy analysis: Bayesian optimization approach
N2 - In materials science, traditional techniques for analyzing layered structures are essential for obtaining information about local structure, electronic properties and chemical states. While valuable, these methods often require high vacuum environments and have limited depth profiling capabilities. The grazing exit x-ray absorption near-edge structure (GE-XANES) technique addresses these limitations by providing depth-resolved insight at ambient conditions, facilitating in situ material analysis without special sample preparation. However, GE-XANES is limited by long data acquisition times, which hinders its practicality for various applications. To overcome this, we have incorporated Bayesian optimization (BO) into the GE-XANES data acquisition process. This innovative approach potentially reduces measurement time by a factor of 50. We have used a standard GE-XANES experiment, which serve as reference, to validate the effectiveness and accuracy of the BO-informed experimental setup. Our results show that this optimized approach maintains data quality while significantly improving efficiency, making GE-XANES more accessible to a wider range of materials science applications.
KW - Machine Learning
KW - GE-XANES
KW - Bayesian Optimization
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603955
DO - https://doi.org/10.1088/2632-2153/ad4253
VL - 5
IS - 2
SP - 1
EP - 12
PB - IOP Publishing
AN - OPUS4-60395
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Coburger, Peter
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Emmerling, Franziska
A1 - Abbenseth, Josh
T1 - Combining geometric constraint and redox non-innocence within an ambiphilic PBiP pincer ligand
N2 - The first pincer ligand featuring a strictly T-shaped pnictogen donor moiety was synthesised. The PBiP ligand's redox activity facilitates unprecedented ambiphilic bonding of the Bi centre with transition metals through the Bi(6p) orbital.
KW - EXAFS
KW - Pincer Ligand
KW - Group 15 metals
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611113
DO - https://doi.org/10.1039/D4SC00197D
SN - 2041-6520
SP - 1
EP - 8
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-61111
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlögl, Johanna
A1 - Goldammer, Ole
A1 - Bader, Julia
A1 - Emmerling, Franziska
A1 - Riedel, Sebastian
T1 - Introducing AFS ([Al(SO3F)3]x) – a thermally stable, readily available, and catalytically active solid Lewis superacid
N2 - This paper introduces the thermally stable, solid Lewis superacid aluminium tris(fluorosulfate) (AFS), that is easy-to-synthesize from commercially available starting materials. Its applicability, e.g. in catalytic C–F bond activations, is shown.
KW - Lewis Acid
KW - C-F activation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601001
DO - https://doi.org/10.1039/D4SC01753F
SN - 2041-6520
SP - 1
EP - 7
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-60100
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Das, Prasenjit
A1 - Chakraborty, Gouri
A1 - Friese, Nico
A1 - Roeser, Jérôme
A1 - Prinz, Carsten
A1 - Emmerling, Franziska
A1 - Schmidt, Johannes
A1 - Thomas, Arne
T1 - Heteropolyaromatic Covalent Organic Frameworks via One-Pot Multicomponent Reactions
N2 - Multicomponent reactions (MCRs) offer a platform to create different chemical structures and linkages for highly stable covalent organic frameworks (COFs). As an illustrative example, the multicomponent Povarov reaction generates 2,4-phenylquinoline from aldehydes and amines in the presence of electron-rich alkenes. In this study, we introduce a new domino reaction to generate unprecedented 2,3-phenylquinoline COFs in the presence of epoxystyrene. This work thus presents, for the first time, structural isomeric COFs produced by multicomponent domino and Povarov reactions. Furthermore, 2,3-phenylquinolines can undergo a Scholl reaction to form extended aromatic linkages. With this approach, we synthesize two thermally and chemically stable MCR-COFs and two heteropolyaromatic COFs using both domino and in situ domino and Scholl reactions. The structure and properties of these COFs are compared with the corresponding 2,4-phenylquinoline-linked COF and imine-COF, and their activity toward benzene and cyclohexane sorption and separation is investigated. The position of the pendant phenyl groups within the COF pore plays a crucial role in facilitating the industrially important sorption and separation of benzene over cyclohexane. This study opens a new avenue to construct heteropolyaromatic COFs via MCR reactions.
KW - COF
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604038
DO - https://doi.org/10.1021/jacs.4c02551
SP - 1
EP - 9
PB - American Chemical Society (ACS)
AN - OPUS4-60403
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wiesner, Yosri
A1 - Hoffmann, Thomas
A1 - Range, David
A1 - Altmann, Korinna
T1 - Microplastics in sediments of the river Rhine—A workflow for preparation and analysis of sediment samples from aquatic river systems for monitoring purposes
N2 - AbstractMicroplastics (MP) can be detected in all environmental systems. Marine and terrestrial aquatic systems, especially the transported suspended solids, have often been the focus of scientific investigations in the past. Sediments of aquatic river systems, on the other hand, were often ignored due to the time‐consuming sample preparation and analysis procedures. Spectroscopic measurement methods counting particle numbers are hardly suitable as detection methods, because there are plenty of natural particles next to a small number of MP particles. Integral methods, such as thermoanalytical methods are determining the particle mass independently of the inorganic components.In this study, a workflow for sample preparation via density separation and subsequent analysis by thermal extraction desorption‐gas chromatography/mass spectrometry is presented, which leads to representative and homogeneous samples and allows fast and robust MP mass content measurements suitable for routine analysis. Polymers were identified and quantified in all samples. Polyethylene and styrene‐butadiene rubber are the dominant polymers, besides polypropylene and polystyrene. Overall, total polymer masses between 1.18 and 337.0 µg/g could be determined. Highest MP concentrations in riverbed sediment are found in sites characterized by low flow velocities in harbors and reservoirs, while MP concentrations in sandy/gravelly bed sediments with higher flow velocities are small.
KW - Microplastics
KW - Density separation
KW - TED-GC/MS
KW - NaI
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597335
DO - https://doi.org/10.1002/appl.202200125
VL - 3
IS - 2
SP - 1
EP - 10
PB - Wiley VHC-Verlag
AN - OPUS4-59733
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Altmann, Korinna
T1 - Seasonal microplastic concentrations along the rivers Rhine and Danube
N2 - Over the last 20 years, many researchers, politicians and citizens have become increasingly aware of the growing plastic problem of our time. A lack of recycling concepts and plastic collection points as well as careless dumping lead to accumulation of plastic products in the environment. Natural weathering can cause these plastics to degrade and fractionate, meaning that microplastics (1 1,000 µm, ISO/TR 21960:2020) and nanoplastics (< 1 µm, ISO/TR 21960:2020) of various synthetic polymer materials can now be detected in all parts of the world. Whether microplastics or nanoplastics pose a toxicological hazard is being investigated in a variety of ways. Valid results are still pending. However, the EU precautionary principle applies to micro- and nanoplastics. Monitoring of microplastics is already required in the revision of the Drinking Water and Wastewater Framework Directive.
Reliable monitoring of rivers can be carried out by sampling with sedimentation boxes and microplastic detection by using thermal extraction desorption gas chromatography/mass spectrometry (TED-GC/MS) in routine operation (Figure 1). The river Rhine was sampled for microplastic masses at three different sampling locations over a period of one year and in addition the Danube at randomized sampling locations The TED-GC/MS results showed that various synthetic polymers frequently produced in industry, such as polyethylene, polypropylene or polystyrene as well as the tire compound styrene-butadiene rubber were found. The work not only shows a possible workflow for monitoring concepts, but also provides information on environmentally relevant concentrations of microplastics and tire components in surface waters. This in turn is necessary for ecotoxicological studies.
T2 - ESOPS
CY - Berlin, Germany
DA - 09.09.2024
KW - Microplastics
KW - TED-GC/MS
KW - Polymer 3R
PY - 2024
AN - OPUS4-61016
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Atanasova, Aleksandra
T1 - Herstellung und Einsatz neuartiger Trypsin-Partikel für den enzymatischen Antikörper-Verdau
N2 - In dieser Arbeit wurden zwei Trypsinvarianten, der Wildtyp (wtT) und eine thermostabile Variante (tsT), rekombinant hergestellt. Die Herstellung von Proteinen in Bakterien kann zu Fehlfaltungen und Einschlusskörperchen führen, weshalb eine geeignete Faltungsstrategie notwendig ist. In dieser Arbeit konnte eine schrittweise Vorgehensweise erfolgreich angewendet werden.
Nach der Ni-NTA-Aufreinigung wurde zusätzlich eine substratspezifische Benzamidin-Aufreinigung eingesetzt, um die Aktivität zu verbessern. Außerdem wurden die rekombinanten Trypsine auf Korund immobilisiert. Korund ist ein kostengünstiges Material, das nach Silanisierung und Glutaraldehyd-Kopplung für die Bindung von Proteinen geeignet gemacht wurde. Dabei konnte gezeigt werden, dass mehr wtT als tsT gebunden wurde, was sich auch in den Kopplungsdichte widerspiegelte.
Die immobilisierten Enzyme wurden in Bezug auf Aktivität, Wiederverwendbarkeit, Lagerfähigkeit und Temperaturstabilität untersucht. Beide Varianten zeigten vergleichbare Leistungen, wobei tsT bei höheren Temperaturen eine etwas bessere Stabilität aufwies. Für den Antikörperverdau wurden sowohl thermische als auch chemische Denaturierungen bei verschiedenen Temperaturen ( 37 °C und 60 °C) getestet. Die Analyse mit MALDI-TOF-MS zeigte, dass gute Werte für die Sequenzabdeckung erzielt werden konnten. Besonders die chemische Denaturierung führte zu besseren Ergebnissen mit weniger Selbstverdau.
Beim Vergleich mit kommerziell immobilisiertem Crude-Trypsin zeigten die rekombinanten Varianten eine höhere Spezifität und bessere Sequenzabdeckung bei gleichzeitig geringerem Selbstverdau. Die Wiederverwendbarkeit wurde durch fünf Verdauzyklen bei 37 °C überprüft. Dabei blieb die Aktivität weitgehend stabil, auch wenn die Peakintensität in den MALDI-Spektren mit jedem Zyklus abnahm. Eine eindeutige Zuordnung der Fingerprints des Antikörpers aus einer Bibliothek von über 90 Antikörpern war trotz dessen gegeben.
KW - Korund
KW - Immobilisierung
KW - Proteomik
KW - Rekombinante Proteine
KW - Thermostabile Enzyme
PY - 2025
SP - 1
EP - 86
CY - Berlin
AN - OPUS4-64433
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Béalu, Zoé
A1 - Walther, Johanna
A1 - Abusafia, Attaallah
A1 - Altmann, Korinna
A1 - Meurer, Maren
A1 - Gretzschel, Oliver
A1 - Schäfer, Michael
A1 - Steinmetz, Heidrun
T1 - Removal of Organic Micropollutants and Microplastics via Ozonation Followed by Granular Activated Carbon Filtration
N2 - Discharge from Wastewater Treatment Plants (WWTPs) can result in the emission of organic micropollutants (OMPs) and microplastics (MPs) into the aquatic environment. To prevent this harmful release, a pilot plant consisting of an ozonation followed by a granular activated carbon (GAC) filter was operated at a WWTP in Germany, and its side-effects on the concentrations of nitrogen (N) and phosphorous (P) compounds were measured. Over 80% of OMPs and transformation products were removed during the operating time (around 6000 bed volumes) no matter the ozone dose (from around 0.1 to 0.5 mgO3/mgDOC), except for Diatrizoic acid, whose breakthrough appeared at 3500 BV. Formation of the oxidation by-product, NDMA, increased with higher ozone doses, but the concentration remained below 100 ng/L. Bromate was formed at a higher ozone dose (0.4 mgO3/mgDOC) but at a low concentration—below 10 µg/L. The MP particles detected in the inflow (PE, SBR, PP, and PS) were effectively eliminated to a high degree, with a removal rate of at least 92%. Carbon parameters (COD, DOC, and SAC254) were removed further by the pilot plant, but to different extents. As expected, nitrate was formed during ozonation, while nitrite’s concentration decreased. Further, nitrite decreased and nitrate increased within the GAC filter, while ammonium was eliminated by at least 90%. Total P concentration decreased after the pilot, but the concentration of PO4-P increased.
KW - Microplastics
KW - TED-GC/MS
KW - Granular Activated Carbon Filtration
KW - Removal of Organic Micropollutants
KW - Wastewater treatment plant
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615209
DO - https://doi.org/10.3390/environments11110241
VL - 11
IS - 11
SP - 1
EP - 38
PB - MDPI AG
AN - OPUS4-61520
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kittner, Maria
A1 - Bauer, Vanessa
A1 - Altmann, Korinna
A1 - Kraft, Oliver
A1 - Nordmann, Thomas
A1 - Kalbe, Ute
T1 - Mikroplastik-Austrage aus Kunststoffrasenplatzen ins Grundwasser
N2 - Sportplätze aus Kunststoffrasen haben sich im Breitensport etabliert, weshalb ihre Anzahl jährlich zunimmt. Dabei werden Umwelt- und Gesundheitsrisiken, insbesondere durch Mikroplastik-Austräge, kontrovers diskutiert. Um die ungenügende Datenlage zur Menge des Austrages an Mikroplastik zu verbessern, haben sich zwei individuelle Studien mit dieser Forschungsfrage mit Fokus auf den Boden-Grundwasser-Pfad befasst, deren Ergebnisse hier erstmalig gemeinsam vorgestellt werden. Die erste Studie simulierte unter Laborbedingungen Mikroplastik-Emissionen von drei Kunststoffrasen-Szenarien in unterschiedlichen Alterungszuständen und analysierte thermoanalytisch. Die zweite Studie untersuchte Grundwasser-Proben von zwei Realsportplätzen, die 1 m unter dem Grundwasserspiegel entnommen und spektroskopisch untersucht wurden. Dies ermöglicht erstmalig einen Vergleich von Mikroplastik-Austrägen über das Sickerwasser in verschiedenen Bodentiefen. Die Labor-Ergebnisse ergaben je nach Alterungszustand des Kunststoffrasenplatzes Mikroplastik-Emissionen zwischen < 0,1 μg/L und 26,8 μg/L in 30 cm Bodentiefe. Wohingegen in den Grundwasser-Proben der Realsportplätze ab 4 m Bodentiefe keine Kunststoffrasen-Partikel detektiert wurden. Dies deutet darauf hin, dass vermehrt Mikroplastik durch Alterung aus Kunststoffrasen entsteht und im Sickerwasser ausgetragen wird, aber der Boden Mikroplastik- Partikel ≥ 5 μm durch Filtrationseffekte zurückhält, sodass diese im Grundwasser nicht nachweisbar waren.
KW - Kunststoffrasen, Alterung, Mikroplastik, Elution, Schadstoffe
PY - 2025
DO - https://doi.org/10.37307/j.1868-7741.2025.04.05
SN - 1868-7741
VL - 30
IS - 4
SP - 156
EP - 161
PB - Erich Schmidt Verlag GmbH & Co. KG
AN - OPUS4-65098
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Altmann, Korinna
A1 - Portela, Raquel
A1 - Barbero, Francesco
A1 - Breuninger, Esther
A1 - Camassa, Laura Maria Azzurra
A1 - Cirkovic Velickovic, Tanja
A1 - Charitidis, Costas
A1 - Costa, Anna
A1 - Fadda, Marta
A1 - Fengler, Petra
A1 - Fenoglio, Ivana
A1 - Giovannozzi, Andrea M.
A1 - Haugen, Øyvind Pernell
A1 - Kainourgios, Panagiotis
A1 - von der Kammer, Frank
A1 - Kirchner, Markus J.
A1 - Lomax-Vogt, Madeleine
A1 - Lujic, Tamara
A1 - Milczewski, Frank
A1 - Moussawi, Mhamad Aly
A1 - Ortelli, Simona
A1 - Parac-Vogt, Tatjana N.
A1 - Potthoff, Annegret
A1 - Reinosa, Julian J.
A1 - Röschter, Sophie
A1 - Sacco, Alessio
A1 - Wimmer, Lukas
A1 - Zanoni, Ilaria
A1 - Dailey, Lea Ann
T1 - Correction: Characterizing nanoplastic suspensions of increasing complexity: Inter-laboratory comparison of size measurements using dynamic light scattering
N2 - Correction for ‘Characterizing nanoplastic suspensions of increasing complexity: Inter-laboratory comparison of size measurements using dynamic light scattering’ by Korinna Altmann et al., Environ. Sci.: Nano, 2025, 12, 5242–5256, https://doi.org/10.1039/D5EN00645G.
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656330
DO - https://doi.org/10.1039/d6en90001a
SN - 2051-8153
VL - 13
IS - 2
SP - 1233
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-65633
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Altmann, Korinna
T1 - Welche Rolle spielen Textilien als Mikroplastik-Quelle im Abwasser?
N2 - In diesem Vortrag wird die Rolle der Waschmaschine als Eintragspfad von Mikroplastik in das Abwasser diskutiert und eine experimentelle Annäherung an das Problem beschrieben.
T2 - Wasserwirtschaftliches Kolloquium der TU Berlin
CY - Berlin, Germany
DA - 14.12.2023
KW - Mikroplastik
KW - TED-GC/MS
KW - Waschmaschine
PY - 2023
AN - OPUS4-59278
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Altmann, Korinna
T1 - Systemverständnis und Untersuchungsstrategien von Kunststoffeinträgen in die Umwelt – Ergebnisse des RUSEKU-Forschungsprojektes
N2 - Ziel des Vortrages ist die Vermittlung der Herausforderungen der Mikroplastik-Analytik sowie der Harmonisierung der Analytik und des Ergebnistransfers in die Normung.
T2 - Jahresabschluss-Sitzung GA "Mensch und Umwelt"
CY - Online meeting
DA - 24.11.2021
KW - Mikroplastik
KW - Mikroplastik-Analytik
PY - 2021
AN - OPUS4-53830
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Altmann, Korinna
T1 - Update from ISO/TC 61/SC14/WG4
N2 - This talk is an update from ISO/TC 61/SC14/WG4. It describes the production of microplastic test material for the use in an interlaboratory comparison. IWe report the first results of an ILC on microplastic detection methods organized under the pre-stantdardisation plattform of VAMAS (www.vamas.org/twa45/) as Project 2 “Development of standardized methodologies for characterisation of microplastics with microscopy and spectroscopy methods”, within the Technical Working Area TWA 45 “Micro and Nano Plastics in the Environment”. The ILC has gathered 84 participants all over the world representing all continents. Reference materials were developed by BAM to test the main methods for MPs detection as addressed in ISO/TR 21960:2020: thermo-analytical methods (Py-GC/MS and TED-GC/MS) and vibrational methods (µ-IR and µ-Raman). As far as the mass fraction is concerned, accurate results with quite a good precision were achieved with the thermo-analytical methods. Number-based results are not adressed here.
T2 - ISO/TC 147/SC 2/JWG
CY - Online meeting
DA - 03.06.2025
KW - Microplastics
KW - ILC
KW - Reference materials
PY - 2025
AN - OPUS4-63340
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Hejazi, Bardia
T1 - X-ray Computed Tomography Image Compression and Denoising with AI
N2 - The ever-growing volume of data in imaging sciences stemming from advancements in imaging technology, necessitates efficient and reliable storage solutions for such large datasets. In this study, we investigated the compression of industrial X-ray computed tomography (XCT) data using deep learning and examined how these compression algorithms affect the quality of the recovered data. To determine best strategies, we investigated two different network architectures with different compression rates. The XCT data used was from a sandstone sample with a complex internal pore network. The quality of the recovered images obtained from the two different deep learning architectures with different compression rates were quantified and compared to the original input data. We showed that the most suitable architecture and compression rate can change, depending on what specific characteristics we would need to preserve for later analysis. The findings presented here can aid scientists in determining the best approaches and strategies for their data storage and analysis requirements.
T2 - BAM AI & ML Symposium
CY - Berlin, Germany
DA - 06.11.2025
KW - X-ray computed tomography
KW - Compression
KW - Deep Learning
PY - 2025
AN - OPUS4-65610
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ciornii, Dmitri
A1 - Hodoroaba, Vasile-Dan
A1 - Wachtendorf, Volker
A1 - Fengler, Petra
A1 - Altmann, Korinna
T1 - Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods
N2 - In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62%−117% (for PE) and 45.9%−62% (for PET). In spectroscopical experiments, the SR varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy.
KW - Microplastics
KW - Interlaboratory comparison
KW - PlasticsFatE
KW - PET
KW - PE
KW - Reference materials
KW - VAMAS
KW - Thermo-analytical methods
KW - Spectroscopical methods
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630462
DO - https://doi.org/10.1021/acs.analchem.4c05403
SN - 1520-6882
VL - 97
SP - 8719
EP - 8728
PB - ACS Publications
AN - OPUS4-63046
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Karafiludis, Stephanos
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Kochovski, Z.
A1 - Feldmann, Ines
A1 - Emmerling, Franziska
A1 - Stawski, Tomasz
T1 - Ni- and Co-Struvites: Revealing Crystallization Mechanisms and Crystal Engineering toward Applicational Use of Transition Metal Phosphates
N2 - Industrial and agricultural waste streams (waste water, sludges, tailings, etc.) which contain high concentrations of NH4+, PO43–, and transition metals are environmentally harmful and toxic pollutants. At the same time, phosphorous and transition metals constitute highly valuable resources. Typically, separate pathways have been considered to extract hazardous transition metals or phosphate independently from each other. Investigations on the simultaneous removal of multiple components have been carried out only to a limited extent. Here, we report the synthesis routes for Ni- and Co-struvites (NH4MPO4·6H2O, M = Ni2+ and Co2+), which allow for P, ammonia, and metal co-precipitation. By evaluating different reaction parameters, the phase and stability of transition metal struvites as well as their crystal morphologies and sizes could be optimized. Ni-struvite is stable in a wide reactant concentration range and at different metal/phosphorus (M/P) ratios, whereas Co-struvite only forms at low M/P ratios. Detailed investigations of the precipitation process using ex situ and in situ techniques provided insights into the crystallization mechanisms/crystal engineering of these materials. M-struvites crystallize via intermediate colloidal amorphous nanophases, which subsequently aggregate and condense to final crystals after extended reaction times. However, the exact reaction kinetics of the formation of a final crystalline product varies significantly depending on the involved metal cation in the precipitation process: several seconds (Mg) to minutes (Ni) to hours (Co). The achieved level of control over the morphology and size makes precipitation of transition metal struvites a promising method for direct metal recovery and binding them in the form of valuable phosphate raw materials. Under this paradigm, the crystals can be potentially up-cycled as precursor powders for electrochemical or (electro)catalytic applications, which require transition metal phosphates.
KW - Crystallization
KW - Struvite
KW - Nickel
KW - Cobalt
KW - Phosphorous recovery
KW - Up-cycling
KW - Aqueous synthesis
PY - 2022
DO - https://doi.org/10.1021/acs.cgd.2c00284
VL - 22
IS - 7
SP - 4305
EP - 4315
PB - ACS Publications
CY - Washington D.C.
AN - OPUS4-55286
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Bartczak, Dorota
A1 - Sikora, Aneta
A1 - Goenaga-Infante, Heidi
A1 - Altmann, Korinna
A1 - Drexel, Roland
A1 - Meier, Florian
A1 - Alasonati, Enrica
A1 - Lelong, Marc
A1 - Cado, Florence
A1 - Chivas-Joly, Carine
A1 - Fadda, Marta
A1 - Sacco, Alessio
A1 - Rossi, Andrea Mario
A1 - Pröfrock, Daniel
A1 - Wippermann, Dominik
A1 - Barbero, Francesco
A1 - Fenoglio, Ivana
A1 - Booth, Andy M.
A1 - Sørensen, Lisbet
A1 - Igartua, Amaia
A1 - Wouters, Charlotte
A1 - Mast, Jan
A1 - Barbaresi, Marta
A1 - Rossi, Francesca
A1 - Piergiovanni, Maurizio
A1 - Mattarozzi, Monica
A1 - Careri, Maria
A1 - Caebergs, Thierry
A1 - Piette, Anne-Sophie
A1 - Parot, Jeremie
A1 - Giovannozzi, Andrea Mario
T1 - Multiparameter characterisation of a nano-polypropylene representative test material with fractionation, light scattering, high-resolution microscopy, spectroscopy, and spectrometry methods
N2 - Reference and quality control materials with comparable physicochemical properties to nanoplastic contaminants present in environmental and food nanoplastics are currently lacking. Here we report a nanoplastic polypropylene material prepared using a top-down approach involving mechanical fragmentation of larger plastics. The material was found to be homogeneous and stable in suspension and has been characterised for average particle size, size distribution range, particle number concentration, polypropylene mass fraction and inorganic impurity Content using a wide range of analytical methods, including AF4, cFFF, PTA, (MA)DLS, MALS, SEM, AFM, TEM, STEM, EDS,Raman, ICP-MS and pyGC-MS. The material was found to have a broad size distribution, ranging from 50 nm to over 200 nm, with the average particle size value dependent on the technique used to determine it. Particle number concentration ranged from 1.7–2.4 × 1010 g−1 , according to PTA. Spectroscopy techniques confirmed that the material was polypropylene, with evidence of aging due to an increased level of oxidation. The measured mass fraction was found to depend on the marker used and ranged between 3 and 5 μg g−1 . Inorganic impurities such as Si, Al, Mg, K, Na, S, Fe, Cl and Ca were also identified at ng g−1 levels. Comparability and complementarity across the measurement methods and techniques is also discussed.
KW - Polypropylene
KW - Nanoplastics
KW - Analytics
KW - Reference material
KW - Scattering methods
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654680
DO - https://doi.org/10.1039/D5EN00917K
SN - 2051-8153
SP - 1
EP - 15
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65468
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Bach, S.
A1 - Visnow, E.
A1 - Panthöfer, M.
A1 - Gorelik, T.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Gulo, A.
A1 - Kolb, U.
A1 - Emmerling, Franziska
A1 - Lind, C.
A1 - Tremel, W.
T1 - Hydrate networks under mechanical stress – A case study for Co3(PO4)2·8H2O
N2 - The nature of the bound water in solids with hydrogen-bonded networks depends not only on temperature and pressure but also on the nature of the constituents. The collapse and reorientation of these network structures determines the stability of hydrated solids and transitions to other crystalline or amorphous phases. Here, we study the mechanochemically induced loss of bound water in Co₃(PO₄)₂·8H₂O and compare this process to the behavior under hydrostatic pressure.
The associated phase transition and its kinetics were monitored by X-ray powder diffraction with Synchrotron radiation and quantitative IR spectroscopy. High shearing forces are responsible for the degradation of the hydrogen-bonded network and the concomitant crystalline–amorphous transformation. UV/Vis spectroscopy, extended X-ray absorption spectroscopy (EXAFS), and X-ray absorption near-edge spectroscopy (XANES) provided information about the short-range order in the amorphous solid, and thermal analysis revealed its composition and showed that the moderate charge densities of the Co²⁺ and PO₄³⁻ ions, which make the hydration enthalpy comparable to the binding energy of the counteranions, and the Formation of hydrogen-bonded networks favor multistage crystallization processes associated with the release and uptake of coordinated water. The changes of the Co²⁺ coordination induce a color change from pink to blue; therefore, Co₃(PO₄)₂·8H₂O can be used as an overheat temperature indicator.
KW - Mechanochemistry
KW - Amorphous materials
KW - Hydrates
KW - Cobalt
KW - Phosphates
PY - 2016
DO - https://doi.org/10.1002/ejic.201501481
SN - 1434-1948
SN - 1099-0682
VL - 2016
IS - 13-14
SP - 2072
EP - 2081
PB - Wiley-VCH Verlag GmbH & Co. KGaA
CY - Weinheim, Germany
AN - OPUS4-36434
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ponader, Marco
A1 - Röder, Bettina
A1 - Paul, Martin
A1 - Weller, Michael G.
T1 - Sintered glass monoliths as supports for affinity columns
N2 - A novel stationary phase for affinity separations is presented. This material is based on sintered borosilicate glass readily available as semi-finished filter plates with defined porosity and surface area. The material shows fast binding kinetics and excellent long-term stability under real application conditions due to lacking macropores and high mechanical rigidity. The glass surface can be easily modified with standard organosilane chemistry to immobilize selective binders or other molecules used for biointeraction. In this paper, the manufacturing of the columns and their respective column holders by 3D printing is shown in detail. The model system protein A/IgG was chosen as an example to examine the properties of such monolithic columns under realistic application conditions. Several specifications, such as (dynamic) IgG capacity, pressure stability, long-term performance, productivity, non-specific binding, and peak shape, are presented. It could be shown that due to the very high separation speed, 250 mg antibody per hour and column can be collected, which surpasses the productivity of most standard columns of the same size. The total IgG capacity of the shown columns is around 4 mg (5.5 mg/mL), which is sufficient for most tasks in research laboratories. The cycle time of an IgG separation can be less than 1 min. Due to the glass material’s excellent pressure resistance, these columns are compatible with standard HPLC systems. This is usually not the case with standard affinity columns, limited to manual use or application in low-pressure systems. The use of a standard HPLC system also improves the ability for automation, which enables the purification of hundreds of cell supernatants in one day. The sharp peak shape of the elution leads to an enrichment effect, which might increase the concentration of IgG by a factor of 3. The final concentration of IgG can be around 7.5 mg/mL without the need for an additional nano-filtration step. The purity of the IgG was > 95% in one step and nearly 99% with a second polishing run.
KW - Affinity Chromatography
KW - Affinity Extraction
KW - Affinity Separation
KW - Protein Purification
KW - Down Stream Processing
KW - Antibody Purification
KW - Diagnostic Antibodies
KW - Therapeutic Antibodies
KW - Automated Purification
KW - HPLC
KW - FPLC
KW - IgG determination
KW - Concentration step
KW - Monoclonal Antibodies
KW - Polyclonal Antibodies
KW - Human Plasma
KW - Glass Support
KW - Borosilicate Glass
KW - Monolith
KW - Sintered Material
KW - Additive Manufacturing
KW - Column holder
KW - Construction
KW - Open Science
KW - Citizen Science
KW - Protein A
KW - Regeneration
KW - High-Speed Separations
KW - Robustness
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527581
DO - https://doi.org/10.3390/separations8050056
SN - 2297-8739
N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M.
VL - 8
IS - 5
SP - 1
EP - 16
PB - MDPI
CY - Basel
AN - OPUS4-52758
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wilke, Manuel
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Reinholz, Uwe
A1 - Rademann, Klaus
A1 - Emmerling, Franziska
T1 - The structure and in situ synthesis investigation of isomorphic mononuclear molecular metal phenylphosphonates
N2 - We describe a fast and effective synthesis for molecular metal phosphonates. Isomorphic compounds [M(II)(HO₃PPh)₂(H₂O₃PPh)₂(H₂O)₂] (M = Mn (1), Co (2), Ni (3); Ph = C₆H₅) were obtained by grinding. The complexes are mononuclear compounds containing neutral and monodeprotonated phenylphosphonic acid and water as ligands. The crystal structures were determined using powder X-ray diffraction (PXRD) data and validated by extended X-ray absorption fine structure (EXAFS) data. Combined synchrotron XRD measurements and Raman spectroscopy were conducted for investigating the reactions in situ. Based on these data, the intermediates were characterized and the formation mechanism was derived.
KW - Mechanochemistry
KW - Metal phosphonate
KW - In situ
KW - XRD
PY - 2016
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-363944
DO - https://doi.org/10.1039/c6dt00787b
SN - 1477-9226
SN - 1477-9234
SN - 1364-5447
VL - 45
IS - 23
SP - 9460
EP - 9467
AN - OPUS4-36394
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wilke, Manuel
A1 - Batzdorf, Lisa
A1 - Fischer, Franziska
A1 - Rademann, Klaus
A1 - Emmerling, Franziska
T1 - Cadmium phenylphosphonates: preparation, characterisation and in situ investigation
N2 - The successful mechanochemical syntheses of three cadmium phenylphosphonates indicates that mechanochemistry is ideally suited for synthesizing metal phosphonates. With this powerful synthesis tool it is possible to synthesize rapidly and efficiently both known and novel phosphonates. The Crystal structures of the two new compounds, and, were solved from PXRD data. They contain monodeprotonated phenylphosphonate and neutral phenylphosphonic acid ligands. The synthesis pathways of all three compounds were investigated in situ. A diffusion mechanism is corroborated by our findings.
Intermediates could be detected and identified. The kinetically favored product (3) could always be detected during the syntheses. The thermodynamic stability of the compounds and the stoichiometric ratio of the starting materials are the two directing factors for the synthesis of the final products.
KW - Mechanochemistry
KW - Metal phosphonate
KW - In situ
KW - MOF
KW - XRD
PY - 2016
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-363322
DO - https://doi.org/10.1039/c6ra01080f
SN - 2046-2069
VL - 6
IS - 42
SP - 36011
EP - 36019
PB - Royal Soc Chemistry
CY - Cambridge, UK
AN - OPUS4-36332
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Reinholz, Uwe
A1 - Riesemeier, Heinrich
A1 - Emmerling, Franziska
T1 - Time- & spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot – new analytical possibilities for in situ material characterization
N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved.
KW - Time resolution
KW - Single-shot XAFS
PY - 2016
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370892
DO - https://doi.org/10.1107/S1600577516003969
SN - 1600-5775
IS - 23
SP - 769
EP - 776
PB - International Union of Crystallography
CY - Chester, UK
AN - OPUS4-37089
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wilke, Manuel
A1 - Klimakow, Maria
A1 - Rademann, K.
A1 - Emmerling, Franziska
T1 - Fast and efficient synthesis of a host guest system: a mechanochemical approach
N2 - An unusually fast and effective synthesis procedure for a host guest system consisting of a metal organic framework (MOF) and a polyoxometalate (POM) is described. The material was synthesised mechanochemically and the evolution of the structure was monitored ex and in situ using synchrotron X-ray diffraction (XRD).
KW - Mechanochemistry
KW - MOF
KW - in situ
PY - 2016
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-354910
UR - http://pubs.rsc.org/en/Content/ArticleLanding/2016/CE/C5CE01868D#!divAbstract
DO - https://doi.org/10.1039/C5CE01868D
VL - 18
IS - 7
SP - 1096
EP - 1100
AN - OPUS4-35491
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Krause, Christina
A1 - Szymoniak, Paulina
A1 - Lohstroh, W.
A1 - Juranyi, F.
A1 - Zamponi, M.
A1 - Frick, B.
A1 - Al-Sabbagh, Dominik
A1 - Emmerling, Franziska
A1 - Zorn, R.
A1 - Schönhals, Andreas
T1 - Complex molecular dynamics of symmetric model discotic liquid crystals: Comparison of Hexakis(hepta-alkanoyloxy)triphenylene (HOT6) with Hexakis(hexa-alkyloxy)triphenylene (HAT6)
N2 - This study investigates the complex molecular dynamics of discotic liquid crystals (DLCs) by comparing two structurally similar compounds: Hexakis(hepta-alkanoyloxy)triphenylene (HOT6) and Hexakis(hexa-alkyloxy)triphenylene (HAT6) having the same triphenyl core and the same length of the alkyl side chain. The difference of both materials is that the alkyl chain is linked by an oxygen bridge to the triphenylene core for HAT6 and by a ester group for HOT6. Using a combination of broadband dielectric spectroscopy, differential scanning calorimetry, X-ray scattering, and neutron scattering techniques, the research explores the glass transition phenomena and relaxation processes in these materials. HOT6, featuring ester linkages, exhibits distinct dynamic behavior compared to HAT6, including two separate glass transitions indicated by the 1- and 2-relaxation found by dielectric spectroscopy which are assigned to the glassy dynamics of the alkyl side chain in the intercolumnar space and that of the columns, respectively. The study reveals that the ester group in HOT6 leads to increased molecular rigidity and altered packing in the intercolumnar space, as evidenced by X-ray scattering and the vibrational density of states. Neutron scattering confirms localized methyl group rotations and a further relaxation process which relates to the -relaxation revealed by dielectric spectroscopy. The findings contribute to a deeper understanding of glassy dynamics in partially ordered systems and highlight the influence of molecular architecture on relaxation behavior in DLCs.
KW - Discotic Liquid Crystals
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655171
DO - https://doi.org/10.1039/d5sm01247c
SN - 1744-6848
SP - 1
EP - 17
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65517
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pavlidis, Sotirios
A1 - Fischer, Eric W.
A1 - Opis-Basilio, Amanda
A1 - Bera, Ayan
A1 - Guilherme Buzanich, Ana
A1 - Álvarez-Sánchez, María
A1 - Wittek, Severin
A1 - Emmerling, Franziska
A1 - Ray, Kallol
A1 - Roemelt, Michael
A1 - Abbenseth, Josh
T1 - Ambiphilic Reactivity and Switchable Methyl Transfer at a T-Shaped Bi(NNN) Complex Enabled by a Redox-Active Pincer Ligand
N2 - We report the transition-metal-like reactivity of a geometrically constrained, ambiphilic bismuth(III) trisamide. Planarization of the Bi(III) center unlocks Bi−C bond formation when reacted with mild electrophiles (alkyl iodides and triflates) accompanied by two-electron oxidation of the utilized NNN pincer nligand. The preservation of the bismuth oxidation state is confirmed by single-crystal X-ray diffraction and X-ray absorption spectroscopy and corroborated by theoretical calculations. Sequential reduction of the oxidized ligand framework alters the reactivity of a generated Bi−Me unit, enabling controlled access to methyl cation, radical, and anion equivalents. The full [Bi(Me)(NNN)]+/•/− redox series was comprehensively characterized using NMR and EPR spectroscopy as well as spectro-electrochemistry. This work represents the first example of ligand-assisted, redox-neutral C−X bond splitting at bismuth, establishing a new paradigm for synthetic bismuth chemistry.
KW - Pincer ligand
KW - XAS
KW - Redox
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654948
DO - https://doi.org/10.1021/jacs.5c18955
SN - 0002-7863
VL - 148
IS - 2
SP - 2683
EP - 2692
PB - American Chemical Society (ACS)
AN - OPUS4-65494
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Chakraborty, Gouri
A1 - Das, Prasenjit
A1 - Bhattacharya, Biswajit
A1 - Prinz, Carsten
A1 - Emmerling, Franziska
A1 - Thomas, Arne
T1 - Room-temperature superprotonic conductivity in COOH-functionalized multicomponent covalent organic frameworks
N2 - In solid materials, the development of hydrogen bonding (H-bonding) networks within pores is crucial for efficient proton conductance. In this study, a chemically stable carboxylic acid-functionalized, quinoline-linked 2D microporous covalent organic framework (COF) (Qy-COOH) was synthesized using the Doebner multicomponent reaction (MCR) and compared to a similar framework lacking the –COOH functionality (Qy-H), prepared via an MC Domino reaction. The proton conductivity of the –COOH-functionalized MCR-COF was significantly enhanced, reaching 10−2 S cm−1, attributed to strong H-bonding interactions between water molecules and the dangling –COOH groups within the COF pores. In contrast, the analogous Qy-H framework exhibited a much lower proton conductivity of 10−5 S cm−1, while an imine-based COF showed only 10−6 S cm−1. This work represents the first demonstration of a general strategy to achieve efficient proton conduction in a class of layered 2D –COOH-functionalized COFs, offering superprotonic conductivity without requiring additives at room temperature. The MCR-COF design approach provides a promising pathway for developing highly stable and high-performance proton-conducting materials.
KW - Multicomponebt
KW - COF
KW - Proton Conductivity
KW - Superprotonic
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653526
DO - https://doi.org/10.1039/D5SC06953J
SN - 2041-6520
SP - 1
EP - 9
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65352
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schmalz, Alina
A1 - Eby, Charles Gaston
A1 - Moss, Caitlin
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Thermally Robust 1D Cu(I) Phosphonate Coordination Polymer Exhibiting Enhanced Proton Conductivity via Humidity‐Driven Pathways
N2 - The development of thermally stable solid-state proton conductors (SSPCs) is crucial for advancing energy-conversion devices such as proton-exchange membrane fuel cells (PEMFCs). In this work, we report the solvothermal synthesis and characterization of a novel, 1D Cu(I) coordination polymer, {Cu(ADP)0.5(BPY)}n (BAM-5), based on anthracenediylphosphonate (H2ADP) and 4,40 -bipyridine (BPY). Single-crystal X-ray diffraction revealed that BAM-5 crystallizes in the triclinic space group P1 and shows a 1D ladder structure connected by the H2ADP and organic BPY linkers, which is assembled into a 2D layer via O−H···O hydrogen bonding interactions between uncoordinated oxygen and the O−H of the phosphonate group. Thermogravimetric and dynamic water sorption analysis demonstrated exceptional thermal robustness of BAM-5 until 230°C and notable water affinity. Proton conductivity measurements found increasing proton conductive properties with increasing temperature and relative humidity.The latter is correlated with the material’s water uptake since the structure itself does not contain any permanent lattice water molecules. A maximum proton conductivity of 6.6 × 10−6 S cm−1 was found at 80°C and 98% RH. To the best of our knowledge, no dense, nonporous 1D coordination polymer without lattice or coordinated solvent molecules has shown comparable proton con� ductivity. The high activation energy suggests a combination of both, a Grotthuss-type proton hopping through the hydrogen� bonded framework, and a vehicular process, in which protons are carried along with absorbed water molecules.
KW - Coordination polymers
KW - Phosphonate ligand
KW - Proton conduction
KW - X-ray diffraction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651382
DO - https://doi.org/10.1002/zaac.202500187
SN - 0044-2313
SP - 1
EP - 8
PB - Wiley VHC-Verlag
AN - OPUS4-65138
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hoque, Maroof Arshadul
A1 - Sommerfeld, Thomas
A1 - Lisec, Jan
A1 - Das, Prasenjit
A1 - Prinz, Carsten
A1 - Heinekamp, Christian
A1 - Stolar, Tomislav
A1 - Etter, Martin
A1 - Rosenberger, David
A1 - George, Janine
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Mechanochemically Synthesized Covalent Organic Framework Effectively Captures PFAS Contaminants
N2 - Per‐ and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants that pose significant health risks, prompting urgent efforts to develop effective removal methods and adsorbers. Covalent organic frameworks (COFs) are metal‐free adsorbers with high stability and tunable porosity. A highly crystalline COF is synthesised mechanochemically using 1,3,5‐tris(4‐aminophenyl)benzene (TAPB) and 1,3,5‐triformylbenzene (TFB). The formation dynamics are monitored in real time with time‐resolved in situ synchrotron X‐ray diffraction. The TAPB‐TFB COF demonstrates good efficiency in eliminating PFAS from water. Perfluorooctanoic acid (PFOA) and perfluorooctanesulfonic acid (PFOS) are effectively extracted, and most of the adsorption occurred within the first 10 min. Additionally, X‐ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and DFT calculations are employed to elucidate the molecular interactions between PFAS and the COF framework. The rapid and efficient removal of PFAS makes TAPB‐TFB COF a promising material for water treatment applications.
KW - COFs
KW - Ball-milling
KW - PFAS
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648712
DO - https://doi.org/10.1002/smll.202509275
SN - 1613-6810
VL - 21
IS - 44
SP - 1
EP - 8
PB - Wiley
CY - Weinheim
AN - OPUS4-64871
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pakrashy, Sourav
A1 - Chakraborty, Souvik
A1 - Manna, Sounik
A1 - Nanda Goswami, Juli
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Mandal, Jishu
A1 - Misra, Sourav
A1 - Maiti Choudhury, Sujata
A1 - Okla, Mohammad K.
A1 - Bose, Adity
A1 - Maurya, Pawan Kumar
A1 - Majhi, Anjoy
A1 - Dolai, Malay
T1 - Inhibition of Human Colorectal Cancer by a Natural Product 7-Acetylhorminone and Interactions with BSA/HSA: Multispectral Analysis and In Silico and In Vitro Studies
N2 - We have semi-synthesized a natural product 7-acetylhorminone from crude extract of Premna obtusifolia (Indian headache tree), which is active against colorectal cancer after probation through computational screening methods as it passed through the set parameters of pharmacokinetics (most important nonblood–brain barrier permeant) and drug likeliness (e.g., Lipinski’s, Ghose’s, Veber’s rule) which most other phytoconstituents failed to pass combined with docking with EGFR protein which is highly upregulated in the colorectal carcinoma cell. The structure of 7-acetylhorminone was confirmed by single crystal X-ray diffraction studies and 1H NMR, 13C NMR, and COSY studies. To validate the theoretical studies, first, in vitro experiments were carried out against human colorectal carcinoma cell lines (HCT116) which revealed the potent cytotoxic efficacy of 7-acetylhorminone and verified preliminary investigation. Second, the drugability of 7-acetylhorminone interaction with serum albumin proteins (HSA and BSA) is evaluated both theoretically and experimentally via steady-state fluorescence spectroscopic studies, circular dichroism, isothermal titration calorimetry, and molecular docking. In summary, this study reveals the applicability of 7-acetylhorminone as a potent drug candidate or as a combinatorial drug against colorectal cancer.
KW - Molecular docking
KW - In situ synthesis
KW - ADMET
PY - 2024
DO - https://doi.org/10.1021/acsabm.4c00335
VL - 7
IS - 5
SP - 3414
EP - 3430
PB - American Chemical Society (ACS)
AN - OPUS4-61114
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Parthasarathy, Thiyagaraj
A1 - Mishra, Manish Kumar
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Ghosh, Soumyajit
T1 - Simultaneously Mechanically Flexible, Photobending, and Acidochromic Cyanostilbene Molecular Crystals
N2 - Molecular crystals that respond to multiple stimuli are gaining significant attention for their potential in smart materials like actuators and sensors. However, imparting multiple stimuli-responsive properties to a single crystal remains a major challenge. Herein, we report two cyanostilbene derivative-based crystals 1 and 2, with various responses to stimuli such as mechanical stress, light, acid vapors, etc. Both crystals 1 and 2 demonstrated mechanical flexibility and reversible acidochromism. Additionally, crystal 1 also exhibited light-induced photobending, which is ascribed to Z to E photoisomerization. Detailed structure–property correlation was established to unravel distinct mechanical responses. The development of these multitasking crystals may find applications in multitasking actuators, anticounterfeiting materials, and more.
KW - Absorption
KW - Crystals
KW - Mechanical flexiblity
KW - Photoisomerization
PY - 2025
DO - https://doi.org/10.1021/acs.cgd.4c01341
VL - 25
IS - 2
SP - 309
EP - 318
PB - American Chemical Society (ACS)
AN - OPUS4-62568
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Michalchuk, Adam
A1 - Emmerling, Franziska
T1 - Time-Resolved InSitu Monitoring of Mechanochemical Reactions
N2 - Mechanochemical transformations offer environmentally benign synthesis routes, whilst enhancing both the speed and selec-tivity of reactions. In this light, mechanochemistry promises to trans-form the way in which chemistry is done in both academia and indus-try but is greatly hindered by a current lack in mechanistic understand-ing. The continued development and use of time-resolved in situ(TRIS) approaches to monitor mechanochemical reactions provides a new dimension to elucidatethese fascinating transformations. We here discuss recent trends in method development that have pushed the boundaries of mechanochemical research. New features of mech-anochemical reactions obtained by TRIS techniques are subse-quently discussed, shedding light on how different TRISapproaches have beenused. Emphasis is placed on the strength of combining complementary techniques. Finally, we outline our views for the po-tential of TRIS methods in mechanochemical research, towards es-tablishing a new, environmentally benign paradigm in the chemical sciences
KW - Mechanochemistry
KW - Material synthesis
KW - Green chemistry
PY - 2022
DO - https://doi.org/10.1002/anie.202117270
SN - 1433-7851
SP - 1
EP - 15
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-54321
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Altmann, Korinna
T1 - Production of small micro- and nanoplastic reference materials supporting harmonization and standardization
N2 - The MICROPLASTICdays at Ljubliana, Slowenia, were organized in cooperation with the PRIORITY cost action. The topic has been reference materials this time.
The talk gives an idea of the preparation of reference materials in micro- and nanoplastic topic to support standardisation and regulation. It defines the term of micro-and nanoplastics and presents different case studies and critical attributes to the production depending on the enduser needs.
T2 - MICROPLASTICdays
CY - Ljubljana, Slovenia
DA - 25.03.2025
KW - Microplastics
KW - Nanoplastics
KW - Reference materials
PY - 2025
AN - OPUS4-62801
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Altmann, Korinna
T1 - Microplastic occurrence in urban sewage systems: Identification of sources for pathways into the environment
N2 - All over the world, microplastic (MP) particles (particle size: 1 - 1.000 µm) are found in water, soil, air, biota and even food products. But plenty of these discussed findings are based on a very low number of real datasets, which are extrapolated to general projections. Furthermore, most data are not comparable because the strategies for sampling, sample preparation and detection methods are not harmonised/ or standardised. This would require extensive proficiancy tests. Because of the ubiquity presence and the unclear risks, which might arise from those particles, various political and environmental organisations (i.e. OECD, UNEP, WHO) identify the reduction of plastic entry in the environment as a key challenge for now and the future. This challenge includes the identification of relevant entry pathways but also the demand of harmonised, meaningful and reliable analytical procedures.
Regarding this task within the last few years, a fast practical solution for MP analysis has been developed, which includes the steps of representative sampling, adequate sample preparation and fast detection. Sampling is done by fractional filtration over sieves with mesh sizes of 500, 100, 50 and 5 µm [1]. The received samples are measured by ThermoExtraction/Desorption-Gas Chromatography-Mass Spectrometry (TED-GC-MS) [1,2]. for the most abundant polymers used in practice, which are polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET), polyamide (PA) and acrylate as well as styrene-butadiene-rubber (SBR), a main component of tires.
The present presentation will give first-time insight in a comprehensive dataset of microplastic analysis for an exemplary urban sewage system. MP mass contents of different waters at several days, such as greywater, stormwater retention tank, influent and effluent of a wastewater treatment plant (WWTP) within an urban sewage system in Germany are determined. Furthermore, the mass of the polymers found in dry weather and rain weather flow are compared. The use of these large datasets allows first expressive conclusions regarding the contribution of urban sewage system to the MP entry sources in the environments.
We found PP and PS in all different waters. Furthermore, there is SBR in influent and also in effluent of the WWTP. Surprisingly, we could also detect hugh amounts of PE in the effluent of the WWTP.
T2 - SETAC Europe 2020
CY - Online meeting
DA - 03.05.2020
KW - Microplastic analysis
KW - TED-GC/MS
KW - Microplastic particles
KW - Microplastic mass contents
PY - 2020
AN - OPUS4-50795
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Bhattacharya, Biswajit
A1 - Akhmetova, Irina
A1 - Rautenberg, Max
A1 - Emmerling, Franziska
T1 - Mechanochemical synthesis of phosphonate-based proton conducting metal organic frameworks and hydrogen-bonded metal phosphonates
N2 - Proton exchange membrane fuel cells (PEMFCs) are one of the most promising alternative green energy technologies that deliver high energy density without CO2 emissions. The proton conductivity of proton exchange membranes (PEM) contributes to the overall efficiency of a PEMFC. Materials being used as PEMs must exhibit high proton conductivity at the working conditions of the targeted PEMFC. To date, Nafion and Nafion-like polymers with acidic functionality are widely used as membrane materials due to their high proton conductivity in the range of 10-1 to 10-2 Scm-1 at higher relative humidity. However, these materials suffer from high costs, hazardous production process, and poor performance at high temperatures, limiting their versatility.
In this context, crystalline porous materials are recognized as promising proton conductors for the proton exchange membrane (PEM) in fuel cell technology, owing to their tunable framework structure. However, it is still challenging bulk synthesis for real-world applications of these materials. Herein, we present mechanochemical gram-scale synthesis of series of mixed ligand metal organic frameworks (MOFs) and metal hydrogen‐bonded organic frameworks (MHOFs) using phenylene diphosphonic acid and 1-hydroxyethylidene-1,1-diphosphonic acid with different bipyridyl type of ligands, respectively. In all cases, the existence of extensive hydrogen bonds with amphiprotic uncoordinated phosphonate hydroxyl and oxygen atoms, the frameworks exhibited high proton conductivity. The study demonstrates the potential of green mechanosynthesis for preparations of framework-based proton conducting materials in bulk scale for green energy generation.
T2 - 4th International Conference on Phosphonate Chemistry, Science and Technology, ICOPHOS-4
CY - Crete, Greece
DA - 02.10.2023
KW - Proton exchange membrane fuel cells
KW - Metal organic frameworks
KW - Proton conducting materials
PY - 2023
AN - OPUS4-58837
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Heinekamp, Christian
T1 - Exploring amorphous lewis-acidic zirconium chloro fluoride as a heterogeneous HF shuttle
N2 - Owing to a growing shortage of fluorspar, a raw material used for producing fluorinated base chemicals, fluorspar has been named among the 30 critical raw materials in the EU. 1 However, the sustainable transfer of fluorine atoms from one molecule to another using heterogeneous catalysts has not yet been reported. Herein, we present the heterogeneous catalyst zirconium chloro fluoride (ZCF) that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
T2 - Make and Measure 2023
CY - Berlin, Germany
DA - 13.09.2023
KW - ZCF
KW - Heterogeneous catalysis
KW - C-F bond activation
KW - HF-shuttle
PY - 2023
AN - OPUS4-59616
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Al-Terkawi, Abdal-Azim
A1 - Prinz, Carsten
A1 - Scholz, Gudrun
A1 - Kemnitz, Erhard
A1 - Emmerling, Franziska
T1 - Ca-, Sr-, and Ba-Coordination polymers based on anthranilic acid via mechanochemistry
N2 - Ca-, Sr-, and Ba-Based coordination polymers (CPs) were prepared mechanochemically by milling metal-hydroxide samples with anthranilic acid (oABAH). {[Ca(oABA)2(H2O)3]}n consists of one-dimensional polymeric chains that are further connected by a hydrogen-bonding network. {[Sr(oABA)2(H2O)2]·H2O}n is a one-dimensional CP in which water molecules bridge Sr2+ ions and increase the dimensionality by building an extended network. {[Ba(oABA)2(H2O)]}n crystallizes as a two-dimensional CP comprising one bridging water molecule. The cation radii influence the inorganic connectivity and dimensionality of the resulting crystal structures. The crystal structures were refined from powder X-ray diffraction data using the Rietveld method. The local coordination environments were studied via extended X-ray absorption fine structure (EXAFS) measurements. The compounds were further characterized using comprehensive analytical methods such as elemental analysis, thermal analysis, MAS NMR, imaging, and dynamic vapor sorption (DVS) measurements. Compounds 1, 2, and 3 exhibit small surface areas which decrease further after thermal annealing experiments. All compounds exhibit a phase transformation upon heating, which is only reversible in 3.
KW - Mechanochemistry
KW - XRD
PY - 2019
DO - https://doi.org/10.1039/c9dt00991d
SN - 1477-9226
SN - 1477-9234
VL - 48
IS - 19
SP - 6513
EP - 6521
PB - Royal Society of Chemistry
AN - OPUS4-48014
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Hoque, Maroof Arshadul
T1 - Mechanochemically synthesized COF for PFAS adsorption
N2 - Since the 1950s, per- and polyfluoroalkyl substances (PFAS) have been widely used in a range of consumer products, including clothing, paints, cookware and fast-food packaging. Properties such as high thermal resistance and water and oil repellency contribute to their wide usage. After decades of production, these substances have eventually found their way into our drinking water. Given the adverse effects of PFAS molecules on human health, the removal of these substances from our drinking water is a matter of urgency.1 This study employs the use of materials known as covalent organic frameworks (COFs) to adsorb PFAS molecules from an aqueous medium. COFs are crystalline, highly porous, two- or three-dimensional polymers with tunable topology and functionalities.² For the purposes of this study, a COF was synthesised using 1,3,5-tris(4-aminophenyl)benzene (TAPB) and 1,3,5-triformylbenzene (TFB) via a mechanochemical process. Mechanochemistry represents a green synthesis method that uses mechanical energy to initiate chemical reactions, as opposed to using harmful solvents and heat.3 Adsorption tests were carried out to test the effectiveness of the material in question against PFAS. The COF was exposed to a solution of perfluorooctanoic acid (PFOA) and perfluorooctanesulfonic acid PFOS). Following a 13-hour period, it was observed that 90% of PFOA and 99% of PFOS had been adsorbed by the COF. Most of the adsorption appeared to have occurred within the first 10 minutes of exposure. It can therefore be concluded that the TAPB-TFB COF is a promising material for the adsorption of PFAS molecules.
T2 - Adlershofer Forschungsforum 2024
CY - Berlin, Germany
DA - 11.11.2024
KW - Covalent organic framework
KW - Mechanochemistry
KW - PFAS
KW - In situ Xray diffraction
PY - 2024
AN - OPUS4-61808
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Stawski, Tomasz
A1 - Karafiludis, Stephanos
A1 - Standl, Jakob
A1 - Ryll, Tom
A1 - Schwab, Alexander
A1 - Prinz, Carsten
A1 - Wolf, Jakob
A1 - Kruschwitz, Sabine
A1 - Emmerling, Franziska
A1 - Völker, Christoph
T1 - High-Entropy Metal Phosphate Synthesis: Advancements through Automation and Sequential Learning Optimization
N2 - To accelerate high-entropy metal phosphate (HEMP) discovery, we employed a Random Forest regression model within a SLAMD framework. Trained on limited initial data, the model efficiently explored the vast compositional space to predict a novel five-metal phosphate, which was then successfully synthesized and validated experimentally.
T2 - AI4 Materials Science and Testing 2025
CY - Berlin, Germany
DA - 06.11.2025
KW - Metal phosphates
KW - High-entropy
KW - Sequential learning
PY - 2025
AN - OPUS4-64686
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Yusenko, Kirill
A1 - Stawski, Tomasz
A1 - Kulow, Anicó
A1 - Cakir, Cafer Tufan
A1 - Röder, Bettina
A1 - Naese, Christoph
A1 - Britzke, Ralf
A1 - Sintschuk, Michael
A1 - Emmerling, Franziska
T1 - BAMline - A real-life sample materials research beamline
N2 - With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research.
KW - Extended X-ray absorption fine structure
KW - Energy storage
KW - Environmental impacts
KW - Nondestructive testing techniques
KW - X-ray fluorescence spectroscopy
KW - Corrosion
KW - Near edge X-ray absorption fine structure spectroscopy
KW - X-ray absorption spectroscopy
PY - 2023
DO - https://doi.org/10.1063/5.0157194
VL - 158
IS - 24
SP - 1
EP - 22
PB - AIP Publishing
AN - OPUS4-57824
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wegner, Karl David
A1 - Häusler, I.
A1 - Knigge, Xenia
A1 - Hodoroaba, Vasile-Dan
A1 - Emmerling, Franziska
A1 - Reiss, P.
A1 - Resch-Genger, Ute
T1 - One-Pot Heat-Up Synthesis of ZnSe Magic-Sized Clusters Using Thiol Ligands
N2 - The synthesis of two new families of ZnSe magic-sized clusters (MSCs) is achieved using the thiol ligand 1-dodecanethiol in a simple one-pot heat-up approach. The sizes of the MSCs are controlled with the thiol ligand concentration and reaction temperature.
KW - ZnSe
KW - Magic-sized cluster
KW - Dodecanethiol
KW - Semiconductor nanocrystals
KW - One-pot synthesis
PY - 2022
DO - https://doi.org/10.1021/acs.inorgchem.2c00041
VL - 61
IS - 19
SP - 7207
EP - 7211
PB - ACS Publications
CY - Washington, DC (USA)
AN - OPUS4-54880
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Misra, Archismita
T1 - Polyoxometalate Ionic Liquids as Protective Coatings for Industrial Infrastructure and Cultural Heritage against Microbiologically Influenced Corrosion (MIC)
N2 - Corrosion of stone and metal due to acid rain and biodeterioration poses significant challenges for industrial and residential infrastructure, as well as cultural heritage, including statues and historical artefacts. A promising mitigation strategy involves thin, transparent films of polyoxometalate-based ionic liquids (POM-ILs) as chemical shields. Stone samples coated with acid-resistant, biocidal POM-ILs exhibited negligible corrosion when exposed to simulated acid rain, in stark contrast to the severe deterioration of unprotected samples. Additionally, their biocidal properties effectively prevent biofilm formation on coated surfaces. Following studies successfully explored the effectiveness of the coating against lampenflora growing in the Pommery Champagne cellar; and the long-term performance of POM-ILs under outdoor environmental conditions. So, POM-ILs have already demonstrated remarkable anticorrosion and antimicrobial properties against aerobic microorganisms and, being water-insoluble, do not leach into aquatic ecosystem. The current research project repurposes the POM-ILs, extending their application to metals, specifically targeting microbiologically influenced corrosion (MIC) in cultural heritage artefacts made of brass, carbon steel, cast iron, and bronze. This involves optimizing nanocoating adhesion to the metal surface and evaluating its protective efficacy against MIC caused by anaerobic microorganisms such as methanogenic archaea and sulfate reducing bacteria (SRB). This presentation will highlight POM-ILs as sustainable, high-performance nanocoatings for biocorrosion mitigation. It will showcase published success stories, discuss ongoing research and proof-of-concept results, and explore future prospects for these advanced materials in safeguarding metal infrastructure and artefacts across different industrial sectors as well as in the context of cultural heritage conservation.
T2 - Euro-MIC COST Action - Closing Workshop Conference
CY - Horsens, Denmark
DA - 17.09.2025
KW - Polyoxometalates
KW - Corrosion
KW - Microbiologically Influenced Corrosion
KW - Ionic Liquid
PY - 2025
AN - OPUS4-64549
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Adhami, Forogh
A1 - Safavi, Maliheh
A1 - Ehsani, Maryam
A1 - Ardestani, Sussan K.
A1 - Emmerling, Franziska
A1 - Simyari, Farzaneh
T1 - Synthesis, crystal structure, and cytotoxic activity of novel cyclic systems in [1,2,4]thiadiazolo[2,3-a]pyridine benzamide derivatives and their copper(ii) complexes
N2 - Three N-(pyridine-2-ylcarbamothioyl)benzamide derivatives were synthesized by the reaction of potassium thiocyanate, benzoyl chloride, and 2-amino pyridine derivatives in one pot. The obtained derivatives were oxidized using copper(II) chloride. During the oxidation, two hydrogen atoms were removed, cyclization of the derivatives occurred, and finally, three new N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives were produced. Coordination of these three new derivative ligands to the copper(II) ion resulted in the formation of three new complexes: dichlorobis(N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide)copper(II), dichlorobis(N-(7-methyl-2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2ylidene)benzamide)copper(II), and dichlorobis(N-(5-methyl-2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide)copper(II). All the synthesized products were characterized by IR, 1H NMR, and 13C NMR spectroscopies. Crystal structures of the obtained N-(pyridine-2-ylcarbamothioyl)benzamide derivatives, N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives, and complexes were determined using X-ray single-crystal diffraction; the positions of atoms, bond lengths, bond angles, and dihedral angles were also determined. In all complexes, the coordination of two large monodentate ligands and two chloride anions to the copper(II) ion resulted in the formation of a stable planar geometry around the central ion. Three N-(pyridine-2-ylcarbamothioyl)benzamide derivatives, three N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives, and three complexes were evaluated for their cytotoxicity against five human cancer cell lines (breast cancer cell line MDA-MB-231, neuroblastoma cell line SK-N-MC, prostate adenocarcinoma cell line LNCap, nasopharyngeal epidermoid carcinoma cell line KB, and liver cancer cell line HEPG-2) using an in vitro analysis. The N-(pyridine-2-ylcarbamothioyl)benzamide derivatives showed no cytotoxic activity, whereas the N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives and their complexes showed significant cytotoxicity, especially against MDA-MB-231 and LNCap cell lines. The complexes demonstrated smaller IC50 values than N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives.
KW - Copper complexes
PY - 2014
DO - https://doi.org/10.1039/c3dt52905c
SN - 1477-9226
VL - 43
IS - 21
SP - 7945
EP - 7957
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65449
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Stawski, Tomasz
T1 - Processing of calcium sulfate in brines
N2 - Calcium sulfate hemihydrate (CaSO4·0.5H2O), also known as bassanite or "plaster of Paris", serves as a precursor for the production of gypsum (dihydrate, CaSO4·2H2O), widely used in construction. Currently, ~200 MT of calcium sulfate are consumed annually.
Bassanite is obtained from gypsum through a solid-state thermal treatment in kilns at temperature ranging from 150 °C to 200 °C. We introduce a more efficient and sustainable method (T < 100 ºC) that enables the direct, rapid, and reversible conversion of gypsum to bassanite using reusable high salinity aqueous solutions (brines with c[NaCl] > 4 M).
These transformations are controlled by the properties of the solution, offering extensive opportunities for precise manipulation of crystal formation and recycling of gypsum waste.
T2 - BESSY User Meeting 2024
CY - Berlin, Germany
DA - 12.12.2024
KW - Gypsum
PY - 2024
AN - OPUS4-62095
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Altmann, Korinna
A1 - Heymann, S.
A1 - Braun, U.
A1 - Bannick, C.-G.
A1 - Heller, C.
A1 - Fuchs, M.
A1 - Scheid, C.
A1 - Abusafia, A.
A1 - Steinmetz, H.
A1 - Ricking, M.
A1 - Kerndorff, A.
T1 - Untersuchungsverfahren von Mikroplastikgehalten im Wasser für Praxis und Wissenschaft
N2 - Zielsetzung des vom Bundesministerium für Bildung und Forschung geförderten Projektes RUSEKU war es, repräsentative Untersuchungsstrategien für die Detektion von Mikroplastik mittels TED GC/MS in wässerigen Medien zu ermitteln. Dabei wurden verschiedene Probenahmekonzepte und – verfahren für unterschiedliche Fallgestaltungen und Fragestellungen untersucht, sowie neue Filtersysteme entwickelt. Bei der Detektion der Partikel lag der Fokus auf der Anwendung und Weiterentwicklung der ThermoExtraktion/Desorption-Gaschromatographie-Massenspektrometrie (TED-GC/MS) zur Bestimmung von Mikroplastikgehalten. Anwendung fanden die Methoden bei der Beprobung von Flaschenwasser, Waschmaschinenabläufen, dem urbanen Abwassersystem der Stadt Kaiserslautern, sowie in Oberflächengewässer.
KW - Mikroplastik
KW - TED-GC/MS
KW - Mikroplastik-Analytik
KW - Probennahme
PY - 2021
VL - 14. Jahrgang
IS - 3
SP - 147
EP - 152
PB - Deutschen Vereinigung für Wasserwirtschaft, Abwasser und Abfall
CY - Hennef
AN - OPUS4-52260
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Eisentraut, Paul
A1 - Altmann, Korinna
T1 - Repräsentative Mikroplastik-Detektion in Umweltproben - Weiterentwicklung der TED-GC/MS
N2 - Die große Herausforderung in der Detektion von Mikroplastik (MP)‑Partikeln (1-1000 µm) besteht darin, sie neben Millionen von natürlichen Partikeln in Umweltproben nachzuweisen. Zum Aufspüren von Senken, Eintragspfaden und für Monitoring-Kampagnen ist ein schnelles, automatisiertes Verfahren unerlässlich. Ein solches Verfahren wurde an der Bundesanstalt für Materialforschung und -prüfung (BAM) mit der ThermoExtraktion/Desorption-Gaschromatographie-Massenspektrometrie (TED-GC/MS) in den letzten Jahren entwickelt.
KW - Mikroplastik
KW - TED-GC/MS
PY - 2021
UR - https://analyticalscience.wiley.com/do/10.1002/was.0004000195
SN - 0016-3538
SP - 2
EP - 5
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-54266
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fahmy, A.
A1 - Saeed, A.
A1 - Dawood, U.
A1 - Abdelbary, H.
A1 - Altmann, Korinna
A1 - Schönhals, Andreas
T1 - Nano-MnO2/xanthan gum composite films for NO2 gas sensing
N2 - Nowadays, sensors based on polymers/nanostructured metal oxide composites have been investigated exten-sively because of their sensitivity to NO2 gas at ambient temperature. In this work, nanocomposite membranes of xanthan gum (XG) with different contents of MnO2 nanoparticles were prepared as a potential NO2 gas sensor operating at room temperature by a simple one-step oxidation-reduction reaction. The structural, morphological, thermal, and electrical properties of the composite membrane were investigated. The FT-IR results confirm the successful preparation of MnO2 through the oxidation of XG by KMnO4 and reveal further the structural changes of the XG/MnO2 nanocomposite upon its exposure to NO2 gas. The capping of the synthesized MnO2 nano-particles by XG, the surface composition of the XG/MnO2 nanocomposite membranes, and the effect of NO2 gas on the surface composition was investigated using the XPS technique. The DC conductivity and dielectric loss of nanocomposites were higher than for neat XG. The conductivities of the nanocomposites XG/MO-4, XG/MO-4/ low NO2, and XG/MO-4/high NO2 composites are half, one, and three orders of magnitude higher than that for pure XG revealing a transition from insulating to conductive properties. The results demonstrated that XG/MnO2 nanocomposite membranes are promising for potential applications in NO2 gas sensing.
KW - Gas sensors
KW - Membranes
KW - Metal oxides
KW - Nanocomposites
KW - Semiconductors
PY - 2022
DO - https://doi.org/10.1016/j.matchemphys.2022.127277
SN - 0254-0584
VL - 296
SP - 1
EP - 14
PB - Elsevier B.V.
AN - OPUS4-56769
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Rautenberg, Max
T1 - Metal phosphonates as proton conductors and ORR catalysts
N2 - Metal phosphonates are promising materials for applications in fuel cells, due to their high proton conductivity and higher chemical and thermal stability compared to the industry standard (e.g. Nafion®). Additionally, metal phosphonates are precursors to porous carbon materials with evenly distributed centers for ORR catalysis. As a fast and sustainable synthesis, mechanochemistry is the synthesis method of choice. Thorough characterization is carried out by XRD, MAS-NMR, XAS, BET, and DVS.
T2 - 2nd European Workshop on Metal Phosphonates
CY - Berlin, Germany
DA - 24.09.2019
KW - Phosphonates
KW - Proton cunductor
KW - Oxygen reduction reaction
KW - Catalysis
KW - Mechanochemistry
PY - 2019
AN - OPUS4-50257
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Prinz, Carsten
A1 - Zimathies, Annett
A1 - Emmerling, Franziska
T1 - Experimental raw data sets associated with certified reference material BAM-P114 (titanium dioxide) for comparison of nitrogen and argon sorption, available in the universal adsorption information format (AIF)
N2 - These data sets serve as models for calculating the specific surface area (BET method) using gas sorption in accordance with ISO 9277.
The present measurements were carried out with nitrogen at 77 Kelvin and argon at 87 Kelvin.
It is recommended to use the following requirements for the molecular cross-sectional area:
Nitrogen: 0.1620 nm²
Argon: 0.1420 nm²
Expected specific surface area for nitrogen (BET): 24 to 25 m²/g
Expected specific surface area for argon (BET): 20 m²/g
Titanium dioxides certified with nitrogen sorption and additionally measured with argon for research purposes were used as sample material.
The resulting data sets are intended to serve as comparative data for own measurements and show the differences in sorption behaviour and evaluations between nitrogen and argon.
These data are stored in the universal AIF format (adsorption information format), which allows flexible use of the data.
KW - Physisorption
KW - Specific surface area
KW - AIF
KW - Argon
KW - Nitrogen
PY - 2024
DO - https://doi.org/10.5281/zenodo.13283291
PB - Zenodo
CY - Geneva
AN - OPUS4-60782
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kraffert, K.
A1 - Kabelitz, Anke
A1 - Siemensmeyer, K.
A1 - Schmack, R.
A1 - Bernsmeier, D.
A1 - Emmerling, Franziska
A1 - Kraehnert, R.
T1 - Nanocasting of superparamagnetic iron oxide films with ordered mesoporosity
N2 - Maghemite and magnetite show superparamagnetic behavior when synthesized in a nanostructured form. The material’s inducible magnetization enables applications ranging from contrast enhancing agents for magnetic resonance imaging to drug delivery systems, magnetic hyperthermia, and separation. Superparamagnetic iron oxides with templated porosity have been synthesized so far only in the form of hard-templated powders, where silicon retained from the template severely degrades the material’s magnetic properties. Here, for the first time, the synthesis of superparamagnetic iron oxides with soft-templated mesopore structure is reported. The synthesis of nanostructured maghemite and magnetite films succeeds using micelles of amphiphilic block-copolymers as templates. A thermal treatment of the initially formed mesoporous ferrihydrite in nitrogen produces maghemite, which can be partly reduced to magnetite via thermal treatment in hydrogen while retaining the templated mesopore structure. The resulting materials feature a unique combination of high surface area, controlled pore diameter, and tunable magnetic properties.
KW - Iron oxide films
KW - Mesoporosity
KW - Soft-templated
PY - 2018
DO - https://doi.org/10.1002/admi.201700960
SN - 2196-7350
VL - 5
IS - 3
SP - 1700960, 1
EP - 1700960, 7
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-43560
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Miclea, P-T
T1 - Evaluation of Toxicological Characteristics of Airborne Nano/Microplastic Particles From the Industrial Environment
N2 - Micro and nano plastic (MNPs) particles and fibres represent a global scale contamination source with hazard potential. They can be identified all around our environment, even in air, soil and water. One of the major global MNPs polluters is the textile industry, which generates plastic particles (nylon, polyester, polyurethane, polyolefin, acrylic etc.) during the manufacturing processes. The study analyses the level of particle concentration outside a company that processes textile yarns, but also from the proximity of workplaces using an online air samplers with cascade and mono filter holders for silicon (Si) and quartz filters, respectively. A laser detector was used for real- time counting of particles of six size classes (PM0.3-PM10). Silicon (Si) filters with a diameter of 9 mm and pore sizes of 10 µm and 1 µm and quartz filters with a diameter of 25 mm and a pore size of 1.2 µm were used for particle sampling. A special holder was designed and made for selective sampling (PM10 and PM1.0) on Si filters. Quartz filters were pre-calcined (8000C) before collection. Sampling parameters: airflow (GilAir Plus pump) -2 l/m3, collection time -3 hours; starting time 7.00 am (T1)/2.00 pm (T2), intermittent natural ventilation, average temperature and humidity: 23.3 0C, RH: 52.5%. The weight of particles collected (µg) on the quart filters was 4.9E-05 (T1) and 5.1E-05 (T2) and on the Si filters 3,2 E-05(T1) and 5E-06(T2). The total number of the outside particles (PM0,3-PM10) was situated between 3584,58 (T1)-15165,05(T2) and inside 9901(T1) and 12921,61(T2). The highest number of PM 10 particles inside was 72/m3 and of PM0.3 particles 71979/m3. The samples were characterized using electron microscopy and µRaman spectroscopy. All samples showed a high concentration of particles on the filter. Samples show only particles with irregular shapes. The equivalent particle diameter was for PM10: 1-5 µm and PM1<1 µm. The total Ion Chromatogram shows the presence of PET-type polymer and the TED GS-MS analysis shows that the weight of the collected particles is PET. After extracting the particles from the quartz filters, they were tested for evaluation of the cytotoxic potential of preparations on human monocyte-macrophage cell cultures and peripheral lymphocytes. In the first case, the level of cytotoxicity was at the border between non-cytotoxic and cytotoxic and in the second test the result was moderate cytotoxic.
T2 - SETAC Europe 2025
CY - Vienna, Austria
DA - 11.05.2025
KW - Microplastics
KW - TED-GC/MS
KW - Nanoplastics
KW - Raman microscopy
PY - 2025
AN - OPUS4-63378
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Pauw, Brian Richard
T1 - NeXus at the core of the HExX-lab
N2 - Through bottom-up, comprehensive digitalisation of all aspects of an experiment, the HEX-lab improves the trustworthiness (traceability, reproducibility, quality) of scientific findings.
The five main parts that make up a materials science experiment, i.e. Sample preparation, Measurements, Processing, Analysis, and Interpretation, each have been addressed in thorough and unique ways in this lab, building up a foundation for a wide range of materials science collaborations. Improvements span the spectrum.
Hardware developments include new sample environments and stages, such as grazing incidence motion towers, electrochemistry cells and flow-through holders, electronic components such as safety interlocks and multipurpose I/O controllers, and liquid handling systems such as coolant flow cross-over systems.
Software developments include:
1) a new comprehensive control system operating on both the RoWaN as well as the MOUSE allowing for full Python control and sequencing of all experimentation,
2) Automated scripts for instrument optimization, sample alignments and measurements,
3) revamped data pipelines and analysis software, standalone or launched as part of operations sequencing dashboards on servers, and
4) meticulously structured archival datafiles, fully documenting sample preparation, measurements, processing and analyses. These allow for holistic databases and dashboards to be constructed to investigate the links between synthesis parameters and resulting morphology.
This presentation will highlight some of the tools and techniques developed and available in the HEX-lab over the years, from sample environments to overarching experiment and data organisation structures.
T2 - Materials Science Core Facility Synergy Forum 2025
CY - Bremen, Germany
DA - 26.02.2025
KW - Digitalization
KW - Automation
KW - HDF5
KW - Traceability
KW - Data stewardship
KW - Lab automation
KW - Holistic science
KW - Methodology
PY - 2025
AN - OPUS4-62676
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Bresch, Harald
T1 - Nano and Advanced Materials - Competences at BAM and perspectives
N2 - This presentation gives an overview about the competencies and the characterization possibilities of nanoparticles at BAT, based on this the development of the OECD TG 125 at BAM. It further describes research activities at BAM concerning the characterization of nanoparticles and the way to the digital representation of these characterization possibilities. It concludes with the challenges of a digital product passport (DPP) for nanomaterial based products and the need of a digital materials passport (DMP). Finally, the activities of BAM are presented which address the former mentioned challenges from ESRP and DPP.
T2 - Austausch Helmholtz Hereon / Digipass & BAM
CY - Berlin, Germany
DA - 07.07.2025
KW - Nanomaterials
KW - ESPR
KW - DPP
KW - Nano
KW - Advanced Materials
PY - 2025
AN - OPUS4-64974
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Smales, Glen Jacob
A1 - Pauw, Brian Richard
T1 - DACHS/MOFs/AutoMOFs_3/Synthesis
N2 - The DACHS (Database for Automation, Characterization and Holistic Synthesis) project aims to create completely traceable experimental data, covering syntheses, measurements, analyses, and interpretations. DACHS_MOFs focuses on the synthesis and characterisation of metal-organic frameworks, across multiple, automation-assisted experimental series (AutoMOFs), with the overall goal of producing reproducible MOF samples through tracking of the synthesis parameters.
DACHS_MOFs is simultaneously used to test the DACHS principles.
This upload contain synthesis data from AutoMOFs_3 in HDF5 format (.h5). Each .h5 file contains detailed information on the chemical, experimenal, and synthesis parameters used during the synthesis of a single AutoMOF sample.
KW - Synthesis
KW - Automation
KW - Traceability
KW - Procedure
PY - 2024
DO - https://doi.org/10.5281/zenodo.11237815
PB - Zenodo
CY - Geneva
AN - OPUS4-60633
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stawski, Tomasz
A1 - Smales, Glen Jacob
A1 - Scoppola, E.
A1 - Jha, D.
A1 - Morales, L. F. G.
A1 - Moya, A.
A1 - Wirth, R.
A1 - Pauw, Brian Richard
A1 - Emmerling, Franziska
A1 - Van Driessche, A. E. S.
T1 - Seeds of imperfection rule the mesocrystalline disorder in natural anhydrite single crystals
N2 - In recent years, we have come to appreciate the astounding intricacies associated with the formation of minerals from ions in aqueous solutions. In this context, a number of studies have revealed that the nucleation of calcium sulfate systems occurs nonclassically, involving the aggregation and reorganization of nanosized prenucleation species. In recent work, we have shown that this particle-mediated nucleation pathway is actually imprinted in the resultant micrometer-sized CaSO4 crystals. This property of CaSO4 minerals provides us with the unique opportunity to search for evidence of nonclassical nucleation pathways in geological environments.
In particular, we focused on large anhydrite Crystals extracted from the Naica Mine in Mexico. We were able to shed light on this mineral's growth history by mapping defects at different length scales. Based on this, we argue that the nanoscale misalignment of the structural subunits, observed in the initial calcium sulfate crystal seeds, propagates through different length scales both in morphological, as well as in strictly crystallographic aspects, eventually causing the formation of large mesostructured single crystals of anhydrite. Hence, the nonclassical nucleation mechanism introduces a “seed of imperfection,” which leads to a macroscopic “single” crystal whose fragments do not fit together at different length scales in a self-similar manner. Consequently, anisotropic voids of various sizes are formed with very welldefined walls/edges. However, at the same time, the material retains in part its single crystal nature.
KW - Calcium sulfate
KW - Anhydrite
KW - Mesocrystal
KW - Nucleation
KW - Naica
PY - 2021
DO - https://doi.org/10.1073/pnas.2111213118
SN - 0027-8424
VL - 118
IS - 48
SP - 1
EP - 11
PB - National Academy of Sciences (USA)
CY - Washington
AN - OPUS4-53820
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wilke, Manuel
A1 - Bach, S.
A1 - Gorelik, T.
A1 - Kolb, U.
A1 - Tremel, W.
A1 - Emmerling, Franziska
T1 - Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution
N2 - Divalent metal phosphonates are promising hybrid materials with a broad field of application. The rich coordination chemistry of the phosphonate linkers enables the formation of structures with different dimensionalities ranging from isolated complexes and layered structures to porous frameworks incorporating various functionalities through the choice of the building blocks.
In brief, metal phosphonates offer an interesting opportunity for the design of multifunctional materials. Here, we provide a short review on the class of divalent metal phosphonates discussing their syntheses, structures, and applications. We present the advantages of the recently introduced mechanochemical pathway for the Synthesis of divalent phosphonates as a possibility to generate new, in certain cases metastable compounds. The benefits of in situ investigation of synthesis mechanisms as well as the implementation of sophisticated methods for the structure analysis of the resulting compounds are discussed.
KW - Metal phosphonate
KW - Mechanochemistry
PY - 2017
DO - https://doi.org/10.1515/zkri-2016-1971
SN - 2194-4946
SN - 2196-7105
VL - 232
IS - 1-3
SP - 209
EP - 222
PB - De Gruyter
AN - OPUS4-40003
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Joester, Maike
A1 - Seifert, Stephan
A1 - Emmerling, Franziska
A1 - Kneipp, Janina
T1 - Physiological influence of silica on germinating pollen as shown by Raman spectroscopy
N2 - The process of silicification in plants and the biochemical
effects of silica in plant tissues are largely unknown. To
study the molecular changes occurring in growing cells
that are exposed to higher than normal concentration of
silicic acid, Raman spectra of germinating pollen grains of
three species (Pinus nigra, Picea omorika, and Camellia
japonica) were analyzed in a multivariate classification
approach that takes into account the variation of biochemical
composition due to species, plant tissue structure,
and germination condition. The results of principal
component analyses of the Raman spectra indicate differences
in the utilization of stored lipids, a changed mobilization
of storage carbohydrates in the pollen grain bodies,
and altered composition and/or structure of cellulose of
the developing pollen tube cell walls. These biochemical
changes vary in the different species.
KW - Silica
KW - Raman spectroscopy
KW - Principal component analysis
PY - 2017
DO - https://doi.org/10.1002/jbio.201600011
SN - 1864-063X
SN - 1864-0648
VL - 10
IS - 4
SP - 542
EP - 552
AN - OPUS4-40090
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Castro, R. A. E.
T1 - New cocrystals of bexarotene with pyridinecarboxamide isomers sustained by the acid∙∙∙aromatic nitrogen supramolecular heterosynthon
N2 - Pharmaceutical cocrystals are homogenous crystalline structures made up of two or more components in a definite stoichiometric ratio, where at least one of the components in the crystal lattice is an active pharmaceutical ingredient (API).1 Pharmaceutical cocrystals have opened the opportunity for engineering solid-state forms designed to have tailored properties to enhance drug product bioavailability and stability, as well a enhance processability of the solid material inputs in drug product manufacture. In this work the cocrystallization of bexarotene, an approved API by the U.S. Food and Drug Administration that belongs to Biopharmaceutics Classification System Class II (low solubility–high permeability), with pyridine carboxamide isomers (picolinamide, nicotinamide and isonicotinamide) was successfully undertaken. The synthesis was achieved by liquid assisted grinding (LAG) and the solids obtained were characterized by differential scanning calorimetry (DSC), infrared spectroscopy (FTIR-ATR), powder X-ray diffraction (XRPD), single crystal X-ray diffraction (SXD), and polarized light thermomicroscopy (PLTM). For bexarotene: picolinamide and bexarotene:isonicotinamide, 1:1 cocrystals were obtained directly from milling. SXD data of bexarotene:isonicotinamide cocrystal reveal acid∙∙∙aromatic nitrogen supramolecular heterosynthon and that the homosynthon amide∙∙∙amide in isonicotinamide is preserved. The bexarotene:nicotinamide mixtures prepared by ball milling give rise to simple binary solid–liquid phase diagram with an eutectic point, well described by the Schröder-van Laar equation. Melt crystallization of the 1:1 mixture gives rise to a cocrystal for which a complex phase behaviour is observed.
T2 - 6th Meeting IAPC
CY - Zagreb, Croatia
DA - 04.09.2017
KW - Crystalline structure
KW - Bexarotene
KW - Powder X-ray diffraction
KW - Single crystal X-ray diffraction
KW - Infrared spectroscopy
PY - 2017
AN - OPUS4-41063
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Nützmann, Kathrin
T1 - Depth dependent phase identification of corrosion zones in ferritic alloys by micro-X-ray absorption near edge structure spectroscopy
N2 - Ferritic steels with chromium contents up to 13 wt% are used as materials for power plant components as boiler materials (< 2 wt% Cr) and super heater tubes (> 9 wt% Cr). These materials are subject to aggressive corrosion caused by hot gases such as CO2, H2O, O2 and SO2. Especially SO2 causes fatal corrosion even as a minor component. To examine sulfurous corrosion mechanisms, experiments with pure SO2 were conducted. A proper analysis of the material changes requires phase identification and quantification with a high lateral resolution within the corrosion scale.
T2 - ANAKON2017
CY - Tübingen, Germany
DA - 03.04.2017
KW - Corosion
KW - Steel
KW - XANES
PY - 2017
AN - OPUS4-40415
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Altmann, Korinna
A1 - Wimmer, Lukas
A1 - Alcolea-Rodriguez, Victor
A1 - Waniek, Tassilo
A1 - Wachtendorf, Volker
A1 - Matzdorf, Kay
A1 - Ciornii, Dmitri
A1 - Fengler, Petra
A1 - Milczewski, Frank
A1 - Otazo-Aseguinolaza, Itziar
A1 - Ferrer, Manuel
A1 - Bañares, Miguel A.
A1 - Portela, Raquel
A1 - Dailey, Lea Ann
T1 - Quality-by-design and current good practices for the production of test and reference materials for micro- and nano-plastic research
N2 - Understanding the environmental and human health impacts of micro- and nanoplastic pollutants is currently a high priority, stimulating intensive methodological research work in the areas of sampling, sample preparation and detection as well as intensive monitoring and testing. It is challenging to identify and quantify microplastics in complex organic matrices and concepts for nanoplastic detection are still in their infancy. All analytical techniques employed in studying micro- and nanoplastics require suitable reference materials for validation measurements, with requirements as diverse as the analytical tools used, ranging from different polymer types, size distributions and shapes of the material to the concentrations employed in different experimental set ups (ng to g amounts). The aim of this manuscript is to outline current good practices for small-scale laboratory production and characterization of suitable test and reference materials. The focus is placed on top-downfragmentation methods as well as bottom-up precipitation methods. Examples using polyethylene, polypropylene, polystyrene and polyethylene terephthalate with size distribution classes of mainly 10–1000, 1–10 and <1 μm particles will be provided. Experiences and suggestions on how to produce well-characterized micro- and nano-plastics for internal research needs will ensure that studies using the materials have robust and informative outcomes.
KW - Mmicroplastics
KW - Nanoplastics
KW - Reference materials
KW - Standard validation method
PY - 2025
DO - https://doi.org/10.1016/j.jhazmat.2025.139595
SN - 0304-3894
VL - 497
SP - 1
EP - 20
PB - Elsevier B.V.
AN - OPUS4-63958
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fischer, Franziska
A1 - Lubjuhn, Dominik
A1 - Greiser, Sebastian
A1 - Rademann, K.
A1 - Emmerling, Franziska
T1 - Supply and demand in the ball mill: competitive cocrystal reactions
N2 - The stability of different theophylline cocrystals under milling conditions was investigated by competitive cocrystal reactions. To determine the most stable cocrystal form under milling conditions, the active pharmaceutical ingredient theophylline was either ground with two similar coformers (benzoic acid, benzamide, or isonicotinamide), or the existing theophylline cocrystals were ground together with a competitive coformer. All competitive reactions were investigated by in situ powder X-ray diffraction disclosing the formation pathway of the milling processes. On the basis of these milling reactions, a stability order (least to most stable) was derived: tp/bs < tp/ba < tp/ina < bs/ina.
KW - Mechanochemistry
KW - Cocrystal
KW - Milling
PY - 2016
DO - https://doi.org/10.1021/acs.cgd.6b00928
SN - 1528-7483
SN - 1528-7505
VL - 16
IS - 10
SP - 5843
EP - 5851
AN - OPUS4-38097
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fischer, Franziska
A1 - Greiser, Sebastian
A1 - Peifer, Dietmar
A1 - Jäger, Christian
A1 - Rademann, K.
A1 - Emmerling, Franziska
T1 - Mechanochemically Induced Conversion of Crystalline Benzamide Polymorphs by Seeding
N2 - Benzamide has been known for its polymorphism for almost 200 years.Three polymorphic forms are described. To date,itwas only possible to crystallizeametastable form in amixture together with the thermodynamically most stable form I. Acomplete transformation of form Iinto the metastable form III by mechanochemical treatment has been achieved. Catalytic amounts of nicotinamide seeds were used to activate the conversion by mechanochemical seeding. NMR experiments indicated that the nicotinamide molecules were incorporated statistically in the crystal lattice of benzamide form III during the conversion. The transformation pathway was evaluated using in situ powder X-ray diffraction.
KW - Nicotinamide
KW - Benzamide
KW - In situ reactions
KW - Mechanochemistry
KW - Polymorphs
PY - 2016
DO - https://doi.org/10.1002/anie.201607358
VL - 128
IS - 46
SP - 14493
EP - 14497
PB - WILEY-VCH
CY - Weinheim
AN - OPUS4-38472
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Emmerling, Franziska
T1 - May the Force be with you - Mechanochemical syntheses studied in situ
N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses.
T2 - Seminar Universität Montpellier
CY - Montpellier, France
DA - 24.01.2019
KW - Mechanochemistry
KW - In situ
PY - 2019
AN - OPUS4-47261
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Wiesner, Yosri
T1 - Reference material candidates for Microplastic analysis
N2 - Microplastic reference material is required for validation and harmonization purposes. This includes the analysis of the pure polymer particles and the validation of the respective measurement methods. In addition, there is the harmonization of different laboratories. On the other hand, sample preparation methods must be validated and harmonized with regard to their recovery and subsequent analysis in the respective matrices. For this purpose, we produce reference material candidates in the form of tablets with different mass fractions and particle numbers of polyethelene terephthalate. In the presentation first measurement results by µ-Raman, µ-FTIR, pyrolysis-GC-MS and TED-GC/MS will be presented.
T2 - SETAC Europe 34th Annual Meeting
CY - Seville, Spain
DA - 05.05.2024
KW - Reference material
KW - Microplastics
KW - PlasticTrace
PY - 2024
AN - OPUS4-60019
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Stawski, Tomasz
T1 - Solution-driven processing of calcium sulfate: the mechanism of the reversible transformation of gypsum to bassanite in brines
N2 - Calcium sulfate hemihydrate (CaSO4ᐧ0.5H2O), also known as bassanite, has been used as a precursor to produce gypsum (dihydrate, CaSO4ᐧ2H2O) for various construction and decorative purposes since prehistoric times. The main route to obtain hemihydrate is a thermal treatment of gypsum at temperatures typically between 150 °C and 200 °C to remove some of the structural water.
In this contribution, we introduce (Fig. 1) a more efficient and sustainable method (T < 100 °C) that enables the direct, rapid, and reversibly conversion of gypsum to bassanite using reusable high salinity aqueous solutions (brines with c[NaCl] > 4 M). The optimum conditions for the efficientproduction 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 typical behaviour of the bassanite phase in low salt environments.
Traditionally, hemihydrate is obtained through a solid state thermal treatment because bassanite is considered to be metastable with respect to gypsum and anhydrite in aqueous solutions, and therefore gypsum-to-bassanite conversion should not occur in water. 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 is 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 structure for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios.
T2 - Granada Münster Discussion Meeting GMDM 10
CY - Münster, Germany
DA - 29.11.2023
KW - Gypsum
KW - Bassanite
KW - Calcium sulfate
KW - Recycling
KW - Scattering
PY - 2024
AN - OPUS4-59162
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - May, Anastasia
T1 - Pyrazinamide-Pimelic Acid Cocrystals: A Mechanochemical and Thermal Study
N2 - Cocrystals represent a promising class of crystalline materials, offering a wide potential for physico-chemical property alteration of chemical compounds, such as their solubility, by cocrystallizing the targeted compound with another solid material. In the present study, we investigated the cocrystal system between the anti-tuberculosis drug pyrazinamide (PZA) and pimelic acid (PA) by thermal characterization and milling conditions of mechanochemical synthesis. Thermal treatment resulted in the formation of a eutectic between the compounds PZA and PA. Furthermore, irreversible separation of the cocrystal occurred upon melting. This finding indicated low stability of the cocrystal and the necessity of mechanochemical synthesis for cocrystal formation. The mechanochemical synthesis parameters were elucidated by investigating the temperature effect while milling and the role of pre-milling the coformer PA using in-situ monitoring techniques. The polymorphism of PA, influenced by temperature and pre-milling, exhibited a substantial impact on the kinetics of cocrystallization. This finding underscores the significance of coformer polymorphism as an additional factor in mechanochemical cocrystallization reactions.
T2 - 11th International Conference on Mechanochemistry and Mechanical Alloying
CY - Berlin, Germany
DA - 14.09.2025
KW - Cocrystal
PY - 2025
AN - OPUS4-65353
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Martins, I.
A1 - Carta, M.
A1 - Haferkamp, Sebastian
A1 - Feiler, Torvid
A1 - Delogu, F.
A1 - Colacino, E.
A1 - Emmerling, Franziska
T1 - Mechanochemical N‑Chlorination Reaction of Hydantoin: In Situ Real-Time Kinetic Study by Powder X‑ray Diffraction and Raman Spectroscopy
N2 - Mechanochemistry has become a valuable tool for the synthesis of new molecules, especially in the field of organic chemistry. In the present work, we investigate the kinetic profile of the chlorination reaction of N-3-ethyl-5,5-dimethylhydantoin (EDMH) activated and driven by ball milling. The reaction has been carried out using 2 mm, 4 mm, 5 mm, 6 mm, and 8 mm ball sizes in a new small custom-made Perspex milling jar. The Crystal structure of the starting material EDMH and the 1-chloro-3-ethyl5,5′-dimethyl hydantoin (CEDMH) chlorination product was solved by single-crystal X-ray diffraction. The reaction was monitored, in situ and in real time, by both powder X-ray diffraction (PXRD) and Raman spectroscopy. Our kinetic data show that the reaction progress to equilibrium is similar at all milling ball sizes. The induction period is very short (between 10 and 40 s) when using 4 mm, 5 mm, 6 mm, and 8 mm balls. For the reaction performed with a 2 mm ball, a significantly longer induction period of 9 min was observed. This could indicate that an initial energy accumulation and higher mixing efficiency are necessary before the reaction starts. Using different kinetic models, we found that the amount of powder affected by critical loading conditions during individual impacts is significantly dependent on the ball size used. An almost linear correlation between the rate of the chemical transformations and the ball volume is observed.
KW - Mechanochemistry
KW - In situ real-time monitoring
KW - N-Chlorination
KW - Kinetics
KW - Hydantoin
KW - Powder X-ray diffraction
KW - Raman spectroscopy
PY - 2021
DO - https://doi.org/10.1021/acssuschemeng.1c03812
VL - 9
IS - 37
SP - 12591
EP - 12601
AN - OPUS4-53541
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Souza, B.
A1 - Chauque, S.
A1 - de Oliveira, P.
A1 - Emmerling, Franziska
A1 - Torresi, R.
T1 - Mechanochemical optimization of ZIF-8/Carbon/S8 composites for lithium-sulfur batteries positive electrodes
N2 - The application of lithium-sulfur (Li-S) batteries is still limited by their rapid capacity fading. The pulverization of the sulfur positive electrode after the lithiation and the consequence dissolution of long chain polysulfides in organic solvents lead to the shuttle effect. To address these issues, here we report the mechanochemical preparation of ZIF-8 (Zeolitic Imidazole Framework-8)-based composites as sulfur hosts for positive electrodes in Li-S batteries. We studied different methods for the incorporation of conductive carbon. Also, the replacement of Zn2+ metal centers by other bivalent metals (Cu2+, Co2+ and Ni2+), enabled the preparation of other ZIF-8-based materials. The positive electrode ZIF-8/C/S8 showed initial discharges of 772 mA h g−1 while the pristine one, ZIF-8/S8, displayed 502 mA h g−1. The enhanced performance of 54% for ZIF-8/C/S8 indicates that the direct mechanochemical synthesis of ZIF-8 with conductive carbon is beneficial at initials charge/discharge process in comparison to traditional slurry preparation (ZIF-8/S8). Also, the Li2S6 absorption tests shows 87% of discoloration with ZIF-8/C/S8, confirming the better polysulfides absorption.
KW - Lithium-sulfur battery
KW - Metal organic frameworks
KW - ZIF-8
KW - Mechanochemistry
PY - 2021
DO - https://doi.org/10.1016/j.jelechem.2021.115459
VL - 896
SP - 115459
PB - Elsevier B.V.
AN - OPUS4-53542
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Stawski, Tomasz
T1 - Seeds of imperfection rule the mesocrystalline disorder in natural anhydrite single crystals
N2 - In recent years, we have come to appreciate the astounding intricacy of the formation process of minerals from ions in aqueous solutions. In this context, a number of studies have revealed that nucleation in the calcium sulfate system is non-classical, involving the aggregation and reorganization of nanosized prenucleation particles. In a recent work we have shown that this particle-mediated nucleation pathway is actually imprinted in the resultant single micron-sized CaSO4 crystals. This property of CaSO4 minerals provides us with an unique opportunity to search for evidence of non-classical nucleation pathways in geological environments. In particular, we focused on the quintessential single crystals of anhydrite extracted from the Naica mine in Mexico. We elucidated the growth history from this mineral sample by mapping growth defects at different length scales. Based on these data we argue that the nano-scale misalignment of the structural sub-units observed in the initial calcium sulfate crystal seed propagate through different length-scales both in morphological, as well as strictly crystallographic aspects, eventually causing the formation of large mesostructured single crystals of anhydrite. Hence, the nanoparticle mediated nucleation mechanism introduces a 'seed of imperfection', which leads to a macroscopic single crystal, in which its fragments do not fit together at different length-scales in a self-similar manner. Consequently, anisotropic voids of various sizes are formed with very well-defined walls/edges. But, at the same time the material retains its essential single crystal nature. These findings shed new light on the longstanding concept of crystal structure.
T2 - S4SAS Conference 2021
CY - Online meeting
DA - 01.09.2021
KW - SAXS
KW - Calcium sulfate
KW - Anhydrite
KW - Mesocrystals
PY - 2021
AN - OPUS4-53630
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Rautenberg, Max
T1 - Fluorine Modified ZIF 8 for Electrochemical Catalysis: Where does the Fluorine go?
N2 - Carbonization of fluorinated metal-organic frameworks (MOFs) should yield fluorinated nitrogen- and metal-doped carbons (F-NMCs), which are a combination of NMCs and fluorinated carbons, each promising electrocatalysts on their own. We synthesized two polymorphs of a fluorinated MOF by mechanical ball mill grinding, and carbonized them to yield potential electrocatalyt materials. The catalytical activity towards the oxygen reduction reaction (ORR) was examined, finding good activites. Simulations from a theoretic model helped assesing the stability of proposed catalytic sites and understanding the measured activites towards the ORR catalysis.
T2 - Online symposium of the CRC 1349 "fluorine-specific interactions"
CY - Online meeting
DA - 29.06.2021
KW - PGM-free catalyst
KW - Oxygen Reduction Reaction
KW - Mechanochemistry
KW - MOFs
KW - Computational chemistry
PY - 2021
AN - OPUS4-53538
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Rautenberg, Max
T1 - Synthesis and characterization of fluorinated Co-Zn-Zeolitic imidazole frameworks for catalysis of the oxygen reduction reaction
N2 - The oxygen reduction reaction (ORR) is a common process in a variety of electrochemical devices, like fuel cells
and metal air batteries. The sluggish kinetics of the ORR require an electrocatalyst to pass this bottleneck.[1]
Currently, the most used catalytical systems are platinum-based, with several drawbacks, such as the high cost,
low availability, and deactivation by CO poisoning.[2] Efforts are made to develop efficient, durable and low cost
catalysts to promote the commercialization of fuel cells.
Non-precious metal catalysts are promising candidates for efficient ORR catalysis. It has been shown that
pyrolyzing metal organic frameworks (MOFs) under inert conditions yields carbon-rich materials, with evenly
distributed metal sites, which possess promising electrocatalytic activity.[3] One widely used type of MOF as ORR
catalyst precursors is the zeolitic imidazole framework (ZIF) where metal cations are linked through imidazolebased ligands.
Herein we report the mechanochemical synthesis, structural analysis and of Co-doped ZIF-8 (Zn), as well as its
fluorinated counterpart Co-doped CF3
-ZIF-8 (Zn). The samples showed electrochemical performance comparable
to platinum after carbonization for 1h at temperatures ranging between 850 – 1000°C.
T2 - 15th International conference on materials chemistry (MC15)
CY - Online meeting
DA - 12.07.2021
KW - PGM-free catalyst
KW - Oxygen Reduction Reaction
KW - Mechanochemistry
KW - MOFs
PY - 2021
AN - OPUS4-53539
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Rautenberg, Max
T1 - The Effect of Fluorine on Catalysts for the Oxygen Reduction Reaction obtained from Metal Organic Frameworks
N2 - The oxygen reduction reaction (ORR) – an important reaction in electrochemical devices, such as fuel cells - is characterized by its sluggish kinetics and therefore requires catalysis. The industry currently relies on platinum as a catalyst, although it is scarce and expensive, hindering the commercial breakthrough of fuel cells in automotive applications. Platinum-free catalysts on basis of nitrogen- and metal doped carbons (NMCs) and fluorinated carbons are promising materials to replace platinum-based catalysts for the ORR. In this work we prepared six metal-organic frameworks (MOFs) by mechanical ball mill grinding and studied their formation by in-situ powder X-ray diffraction. Furthermore, the samples were carbonized under controlled conditions (900°C, 1h, N2-atmosphere) to yield carbon materials, that were employed in ORR-electrocatalysis. The effect of Co-doping and fluorination was systematically studied and outstanding ORR activity was found for the catalyst prepared from the Co-doped fluorinated ZIF-8.
T2 - International Symposium on Fluorine-specific interactions
CY - Berlin, Germany
DA - 27.09.2021
KW - PGM-free catalyst
KW - Oxygen Reduction Reaction
KW - Mechanochemistry
KW - MOFs
PY - 2021
AN - OPUS4-53533
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Rautenberg, Max
T1 - Fluorination and co-doping of ZIF-8 by ball mill grinding for efficient oxygen reduction electrocatalysis
N2 - The oxygen reduction reaction (ORR) is a common process in a variety of electrochemical devices, like fuel cells and metal air batteries. The sluggish kinetics of the ORR require an electrocatalyst to pass this bottleneck.[1] Currently, the most used catalytical systems are platinum-based, with several drawbacks, such as the high cost, low availability, and deactivation by CO poisoning.[2] Efforts are made to develop efficient, durable and low cost catalysts to promote the commercialization of fuel cells.
Non-precious metal catalysts are promising candidates for efficient ORR catalysis. It has been shown that pyrolyzing metal organic frameworks (MOFs) under inert conditions yields carbon-rich materials, with evenly distributed metal sites, which possess promising electrocatalytic activity.[3] One widely used type of MOF as ORR catalyst precursors is the zeolitic imidazole framework (ZIF) where metal cations are linked through imidazole-based ligands. Their porous nature is partially retained after carbonization, making MOFs very suitable precursor materials.
Herein we report the mechanochemical synthesis and structural analysis of Co-doped ZIF-8 (Zn), as well as two polymorphs (dense and prorous) of fluorinated Co-doped CF3-ZIF-8 (Zn). The samples showed electrochemical performance comparable to platinum after carbonization for 1 h at temperatures ranging between 850 – 1000°C.
T2 - XXV General Assembly and Congress of the International Union of Crystallography - IUCr 2021
CY - Prague, Czech Republic
DA - 14.08.2021
KW - PGM-free catalyst
KW - Oxygen Reduction Reaction
KW - Mechanochemistry
KW - MOFs
PY - 2021
AN - OPUS4-53535
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Linberg, Kevin
T1 - Tipping the Energy Scales to Control Mechanochemical Polymorphism
N2 - Control of ball milling conversions is required before the full potential of mechanochemical processing can be realized. It is well known that many parameters affect the outcome of mechanochemical polymorphism, but the energy of ball milling itself is often overlooked. We show here how this parameter alone can exert a significant influence on the polymorphic outcome of ball mill grinding by allowing the selective isolation of two polymorphic forms in their pure form under the same grinding conditions. Furthermore, we show how apparent mechanochemical equilibria can be deceptive. Our results clearly demonstrate the need for careful design and interpretation of ball milling experiments beyond current thinking.
T2 - SALSA make and measure
CY - Online meeting
DA - 16.09.2021
KW - Mechanochemistry
KW - Energy
KW - Polymorph
KW - Cocrystal
PY - 2021
AN - OPUS4-53293
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Breßler, Ingo
A1 - Kohlbrecher, J.
A1 - Thünemann, Andreas
T1 - SASfit: a tool for small-angle scattering data analysis using a library of analytical expressions
N2 - SASfit is one of the mature programs for small-angle scattering data analysis and has been available for many years. This article describes the basic data processing and analysis workflow along with recent developments in the SASfit program package (version 0.94.6). They include (i) advanced algorithms for reduction of oversampled data sets, (ii) improved confidence assessment in the optimized model parameters and (iii) a flexible plug-in system for custom user-provided models. A scattering function of a mass fractal model of branched polymers in solution is provided as an example for implementing a plug-in. The new SASfit release is available for major platforms such as Windows, Linux and MacOS. To facilitate usage, it includes comprehensive indexed documentation as well as a web-based wiki for peer collaboration and online videos demonstrating basic usage. The use of SASfit is illustrated by interpretation of the small-angle X-ray scattering curves of monomodal gold nanoparticles (NIST reference material 8011) and bimodal silica nanoparticles (EU reference material ERM-FD-102).
KW - Small-angle X-ray scattering
KW - Small-angle neutron scattering
KW - Curve fitting
KW - Nanotechnology
KW - Nanoparticles
KW - Polymers
KW - SAXS
PY - 2015
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-343348
DO - https://doi.org/10.1107/S1600576715016544
SN - 0021-8898
SN - 1600-5767
VL - 48
SP - 1587
EP - 1598
PB - Blackwell
CY - Oxford
AN - OPUS4-34334
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Breßler, Ingo
A1 - Pauw, Brian Richard
A1 - Thünemann, Andreas
T1 - McSAS: software for the retrieval of model parameter distributions from scattering patterns
N2 - A user-friendly open-source Monte Carlo regression package (McSAS) is presented, which structures the analysis of small-angle scattering (SAS) using uncorrelated shape-similar particles (or scattering contributions). The underdetermined problem is solvable, provided that sufficient external information is available. Based on this, the user picks a scatterer contribution model (or 'shape') from a comprehensive library and defines variation intervals of its model parameters. A multitude of scattering contribution models are included, including prolate and oblate nanoparticles, core-shell objects, several polymer models, and a model for densely packed spheres. Most importantly, the form-free Monte Carlo nature of McSAS means it is not necessary to provide further restrictions on the mathematical form of the parameter distribution; without prior knowledge, McSAS is able to extract complex multimodal or odd-shaped parameter distributions from SAS data. When provided with data on an absolute scale with reasonable uncertainty estimates, the software outputs model parameter distributions in absolute volume fraction, and provides the modes of the distribution (e.g. mean, variance etc.). In addition to facilitating the evaluation of (series of) SAS curves, McSAS also helps in assessing the significance of the results through the addition of uncertainty estimates to the result. The McSAS software can be integrated as part of an automated reduction and analysis procedure in laboratory instruments or at synchrotron beamlines.
KW - Nanotechnology
KW - Nanoparticles
KW - Small-angle X-ray scattering
KW - SAXS
PY - 2015
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-334396
DO - https://doi.org/10.1107/S1600576715007347
SN - 0021-8898
SN - 1600-5767
VL - 48
IS - 3
SP - 962
EP - 969
PB - Blackwell
CY - Oxford
AN - OPUS4-33439
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - INPR
A1 - Pauw, Brian Richard
A1 - Laskina, Sofya
A1 - Naik, Aakash
A1 - Smales, Glen Jacob
A1 - George, Janine
A1 - Breßler, Ingo
A1 - Benner, Philipp
T1 - "Ultima Ratio": Simulating wide-range X-ray scattering and diffraction
N2 - We demonstrate a strategy for simulating wide-range X-ray scattering patterns, which spans the small- and wide scattering angles as well as the scattering angles typically used for Pair Distribution Function (PDF) analysis. Such simulated patterns can be used to test holistic analysis models, and, since the diffraction intensity is on the same scale as the scattering intensity, may offer a novel pathway for determining the degree of crystallinity.
The "Ultima Ratio" strategy is demonstrated on a 64-nm Metal Organic Framework (MOF) particle, calculated from Q < 0.01 1/nm up to Q < 150 1/nm, with a resolution of 0.16 Angstrom. The computations exploit a modified 3D Fast Fourier Transform (3D-FFT), whose modifications enable the transformations of matrices at least up to 8000^3 voxels in size. Multiple of these modified 3D-FFTs are combined to improve the low-Q behaviour. The resulting curve is compared to a wide-range scattering pattern measured on a polydisperse MOF powder. While computationally intensive, the approach is expected to be useful for simulating scattering from a wide range of realistic, complex structures, from (poly-)crystalline particles to hierarchical, multicomponent structures such as viruses and catalysts.
KW - X-ray
KW - Simulation
KW - 3D Fourier Transform
KW - High resolution
KW - XRD
KW - SAXS
KW - PDF
KW - Total scattering
KW - X-ray scattering
KW - Metal organic framework
KW - Electron density map
KW - FFT
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572067
DO - https://doi.org/10.48550/arXiv.2303.13435
VL - Cornell University
SP - 1
EP - 12
PB - Ithaca, NY
AN - OPUS4-57206
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -