Chemische Charakterisierung und Spurenanalytik
Filtern
Dokumenttyp
- Vortrag (90)
- Zeitschriftenartikel (72)
- Posterpräsentation (27)
- Forschungsdatensatz (3)
- Forschungsbericht (2)
- Buchkapitel (1)
- Beitrag zu einem Tagungsband (1)
- Sonstiges (1)
Sprache
- Englisch (156)
- Deutsch (40)
- Mehrsprachig (1)
Schlagworte
- Synchrotron (33)
- BAMline (30)
- Mikroplastik (29)
- TED-GC/MS (25)
- Microplastic (18)
- Microplastics (18)
- XRF (18)
- Mechanochemistry (10)
- TED-GC-MS (9)
- XANES (9)
- MALDI-TOF MS (8)
- Gold (7)
- Machine learning (7)
- Nanoparticle (6)
- Reference material (6)
- Analytik (5)
- Polymer 3R (5)
- XRD (5)
- Analysis (4)
- Automation (4)
- Bayesian Statistics (4)
- In situ (4)
- Pollen (4)
- Polylactide (4)
- Reference materials (4)
- Single cell analysis (4)
- TXRF (4)
- Water (4)
- Archaea (3)
- Coded Aperture (3)
- DNA (3)
- Dosimetry (3)
- Gaussian process (3)
- Machine Learning (3)
- Microbiologically influenced corrosion (3)
- Mikroplastik-Analytik (3)
- Nanoparticles separation capillary electrophoresis asymmetrcial flow field flow fractionation (3)
- Neural network (3)
- Probennahme (3)
- Referenzmaterialien (3)
- SAXS (3)
- Sampling (3)
- Sampling techniques (3)
- Standardisation (3)
- Tire wear (3)
- Trinkwasser (3)
- Affinity Chromatography (2)
- Aktivkohle (2)
- Amperometry (2)
- Analytic (2)
- Artificial Inelligence (2)
- Artificial intelligence (2)
- Asymmetrical flow field flow fractionation (AF4) (2)
- Batteries (2)
- Bayesian Optimization (2)
- Bioimaging (2)
- CXC (2)
- Capillary electrophoresis (2)
- Capillary electrophoresis (CE) (2)
- Certification (2)
- Crystalinity (2)
- D2XRF (2)
- EXAFS (2)
- FPLC (2)
- HPLC (2)
- Harmonisation (2)
- Homogeneity (2)
- ILC (2)
- Immunoassay (2)
- Internal Standard (2)
- Ionization (2)
- Lanthanide (2)
- MALDI TOF MS (2)
- Nanomaterial (2)
- Polymere (2)
- Polymers (2)
- Probenahme (2)
- Quality testing (2)
- Referenzmaterial (2)
- Risk assessment (2)
- SC-ICP-ToF-MS (2)
- Sc-ICP-ToF-MS (2)
- Soil (2)
- Spectroscopy (2)
- Stability (2)
- Standarisierung (2)
- Synthesis (2)
- Thermogravimetrie (2)
- Umwelt (2)
- Wasseraufbereitung (2)
- X-ray fluorescence (2)
- XAFS (2)
- A4F (1)
- AG nanoparticle (1)
- AU nanoparticle (1)
- Absorption spectrometry (1)
- Acidic oxygen evolution reaction (1)
- Acoustic levitation (1)
- Acute myocardial infarction (1)
- Additive (1)
- Additive Manufacturing (1)
- Affinity Extraction (1)
- Affinity Separation (1)
- Amyloid (1)
- Analyse (1)
- Analytical Sciences (1)
- Analytical standards (1)
- Antibodies (1)
- Antibody Purification (1)
- Antikensammlung Berlin (1)
- Application properties (1)
- Archaeometry (1)
- Archäometrie (1)
- Artificial Intelligence (1)
- Aspergillus (1)
- Atomic layer deposition (1)
- Aufbereitung (1)
- Automated Purification (1)
- Barium (1)
- Battery (1)
- Bayes (1)
- Bbeverages (1)
- Beamline (1)
- Bernstorf (1)
- Biological & biomedical applications (1)
- Biomarker (1)
- Biosensor (1)
- Biosynthesis (1)
- Bismuth (1)
- Bisphenol A (1)
- Bone matrix (1)
- Borosilicate Glass (1)
- Böden (1)
- CCQM key comparison (1)
- Calcium monofluoride (1)
- Carboxyl group (1)
- Cardiac troponin (1)
- Cascade filtration (1)
- Catalysts (1)
- Cathode material (1)
- Causes leading to scientific misconduct (1)
- Channel access (1)
- Chemical composition (1)
- Chemical transformation (1)
- Chemiluminescence (1)
- Citizen Science (1)
- Classification (1)
- Cobalt deposition (1)
- Cocoa (1)
- Cocrystal (1)
- Color X-ray Camera (1)
- Column holder (1)
- Comparative test (1)
- Compost (1)
- Concentration step (1)
- Conjugate (1)
- Construction (1)
- Coordination polymers (1)
- Core-shell nanoparticles (1)
- Core/shell nanoparticle (1)
- Corrosion (1)
- Coupling reactions (1)
- Crystallization (1)
- Cyclic voltammetry (1)
- Cyclization (1)
- Cycloparaphenylenes (1)
- Cylic Voltammetry (1)
- DNA strand break (1)
- Data conversion (1)
- Data manipulation (1)
- Debye-Waller parameter (1)
- Deep work (1)
- Degradation (1)
- Density separation (1)
- Depth profile (1)
- Desorption (1)
- Detektion (1)
- Detektion von Mikroplastik (1)
- Diagnosis (1)
- Diagnostic Antibodies (1)
- Digital laboratory (1)
- Digitalization (1)
- Dispersive-XAS (1)
- Dose (1)
- Down Stream Processing (1)
- EPICS (1)
- Ectoine (1)
- Ectoine radiation protection (1)
- Egypt (1)
- Electrocatalysis (1)
- Electrochemistry (1)
- Electrohpresis (1)
- Elektronenmikroskopie (1)
- Emergency (1)
- Endocrine disruptor (1)
- Energy input (1)
- Energy storage (1)
- Environmental analysis (1)
- Environmental impacts (1)
- Epoxy (1)
- Extended X-ray absorption fine structure (1)
- FTIR (1)
- Farbenlehre (1)
- Fenton (1)
- Filter crucible (1)
- Filtration (1)
- Flow injection immunoassay (1)
- Fluorescence (1)
- Fluorine (1)
- Folic acid (1)
- Food safety (1)
- Fraktionierte Filtration (1)
- Framework (1)
- Fundamentals (1)
- Fusarium (1)
- GUI (1)
- Gaussian Process (1)
- General Chemistry (1)
- General Materials Science (1)
- Gilding (1)
- Glass (1)
- Glass Support (1)
- Goethe (1)
- Graphite furnace (1)
- Greek curse tablets (1)
- H/D-Austausch (1)
- H/D-Exchange (1)
- H2020 (1)
- HDF5 (1)
- HERFD-XAS (1)
- HR-CS-MAS (1)
- Hamonisierung (1)
- Handheld (1)
- Harmonisierung (1)
- Hazardous substances (1)
- Heart attack (1)
- Heavy metals (1)
- Hierarchical cluster analysis (1)
- High repetition-rate (1)
- High-Speed Separations (1)
- High-entropy alloy (1)
- High-resolution synchrotron XRF (1)
- Histology (1)
- Holistic science (1)
- Host–guest systems (1)
- Human Plasma (1)
- Hydrogen (1)
- ILC on detection methods (1)
- IgG determination (1)
- Image manipulation (1)
- Immuno assay (1)
- Immunometric assay (1)
- Immunometric biosensor (1)
- Immunosensor (1)
- Implant material (1)
- In situ EXAFS (1)
- In situ SAXS/WAXS (1)
- In situ studies (1)
- Inlet ionization (1)
- Instrument control (1)
- Instrumentation (1)
- Instrumentation utilization (1)
- Inter-laboratory comparison (1)
- Interner Standard (1)
- Ion mobility (1)
- Ionizing radiation (1)
- Iridium oxide (1)
- Klassifizierung (1)
- LA-ICP-MS (1)
- Laboratory automation (1)
- Laboratory management (1)
- Lacunary Keggin ion (1)
- Lead ions (1)
- Lead isotopes (1)
- Levitation (1)
- Li-ion battery (1)
- Luminol (1)
- MALDI (1)
- MALDI Imaging (1)
- MALDI Imaging MS (1)
- MALDI-TOF Massenspektrometrie (1)
- MALDI-ToF MS (1)
- MAS NMR spectroscopy (1)
- MCC (1)
- MDG ICP-ToF-MS (1)
- MOF (1)
- MOUSE (1)
- Machining (1)
- Macrocycles (1)
- Macrophagen (1)
- Magnetic nanocatalyst (1)
- Maia detector (1)
- Mass contents (1)
- Mass spectrometry (1)
- Massenspektrometrie (1)
- Material characterization (1)
- Matrices (1)
- Measurement data conversion (1)
- Mechanism (1)
- Mechanochemical synthesis (1)
- Metal nanoparticles (1)
- Metal-tag (1)
- Metformin (1)
- Methodenentwicklung Böden (1)
- Methodology (1)
- Metrics (1)
- Microdosimetry (1)
- Microdroplet generator (1)
- Microfluidic system (1)
- Microplastic analysis (1)
- Microplastic mass (1)
- Microplastic particles (1)
- Microplastic pathways (1)
- Microplastics analytic (1)
- Microplastics detection (1)
- Microplastics sampling (1)
- Microplastics standardisation (1)
- Mikroplastik Böden (1)
- Mikroplastik Massegehalt (1)
- Mikroplastik in Luft (1)
- Mikroplastikreferenzmaterial (1)
- Modelling (1)
- Molecular recognition (1)
- Molecule (1)
- Monitoring (1)
- Monoclonal Antibodies (1)
- Monoclonal antibodies (1)
- Monolith (1)
- Monolithic column (1)
- Motor controller (1)
- Multimodal (1)
- Multivariate Analyse (1)
- Multivariate Statistics (1)
- Multivariate analyses (1)
- Mycotoxin (1)
- Mycotoxins (1)
- NIR spectroscopy (1)
- NMR (1)
- NXsas (1)
- Nano (1)
- Nanocarrier (1)
- Nanocrystal (1)
- Nanomaterials (1)
- Nanoparticles (1)
- Nanoparticles with same nominal diameter (1)
- Nanoparticles with same nominal diameter; surface coating; two-dimensional off-line coupling (1)
- Nanoplastic (1)
- Nanoplastics (1)
- Natural language processing (1)
- NeXus (1)
- Near edge X-ray absorption fine structure spectroscopy (1)
- Nebra (1)
- Neural Network (1)
- Neural networks (1)
- Nondestructive testing techniques (1)
- OECD (1)
- Ochratoxin A (1)
- Online biosensor (1)
- Open Science (1)
- Optimierung (1)
- Outreach (1)
- P-aminothiophenol (1)
- PET (1)
- PXRD (1)
- Paper mills (1)
- Partial least square discriminant analysis (PLS-DA) (1)
- Particle size distribution (1)
- Pb isotopes (1)
- Peroxidase (1)
- Pharmacy (1)
- Phosphonate esters (1)
- Phosphonates (1)
- Photocatalysis (1)
- Photodegradation (1)
- Photooxidation (1)
- Plastic bottles (1)
- Pollen grains (1)
- Pollenkörner (1)
- Polycapillaries (1)
- Polyclonal Antibodies (1)
- Polyethyleneglycol (1)
- Polymer blends (1)
- Polymere Eigenschaften (1)
- Polymorph (1)
- Polymorphs (1)
- Polyoxometalates (1)
- Polyurethanes (1)
- Pomodore (1)
- Poster presentation (1)
- Principal component analysis (1)
- Principal component analysis (PCA) (1)
- Prisma (1)
- Probenpräparation (1)
- Procedure (1)
- Protein A (1)
- Protein Purification (1)
- Purification (1)
- Purity assessment (1)
- Python (1)
- Quality (1)
- Qualitätssicherung (1)
- Quantum dot (1)
- Quick-XAS (1)
- RUSEKU (1)
- RXES (1)
- Radiation (1)
- Radiation damage (1)
- Raman (1)
- Refractory alloys (1)
- Regeneration (1)
- Reifenabrieb (1)
- Release kinetics (1)
- Reliabiilty (1)
- Renewable Energy (1)
- Rhizopus (1)
- Ringversuch (1)
- Ringversuche (1)
- River (1)
- Robustness (1)
- Röntgenfluoreszenz (1)
- Salt (1)
- Sample preparation (1)
- Sata corrections (1)
- Scattering (1)
- Scientific misconduct (1)
- Sedimentation box (SB) (1)
- Sedimentationskasten (1)
- Sedimenttaionskasten (1)
- Self-assembly (1)
- Sensing (1)
- Separation (1)
- Sers (1)
- Si wafer filter (1)
- Silver nanoparticles (1)
- Sintered Material (1)
- Size (1)
- Size exclusion chromatography (1)
- Slags (1)
- Small-angle scattering (1)
- Soft-templated mesoporous films (1)
- Software (1)
- Solid support (1)
- Solvent-free (1)
- Sonochemical synthesis (1)
- Spinel (1)
- Sportböden (1)
- Supramolecular chemistry (1)
- Surface chemistry (1)
- Surface coating (1)
- Suspended particulate matter (SPM) (1)
- Sustainability and the Environment (1)
- TGA-FTIR (1)
- TGA-MS (1)
- TMB (1)
- TXRF-XAS (1)
- Tattoo inks (1)
- Temperature (1)
- Tesserae (1)
- Textile fibres (1)
- The MOUSE (1)
- Therapeutic Antibodies (1)
- Thermal analysis (1)
- Thermal degradation (1)
- Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), monitoring (1)
- Thermal extraction-desorption gas chromatography mass spectrometry (1)
- Thermo-desorption (1)
- Thermoanalyse (1)
- Thermoanalysis (1)
- Thermoanalytic (1)
- Thermoanalytical methods (1)
- Thermoanalytics (1)
- Thermoanalytik (1)
- Tire Wear (1)
- Tire particles (1)
- Tools to combat scientific misconduct (1)
- Toxic metals (1)
- Traceability (1)
- Transesterification (1)
- Two-dimensional off-line coupling (1)
- Ultrasound (1)
- Underwater LIBS (1)
- Urban (1)
- VAMAS (1)
- VRF (1)
- Vacuum ionization (1)
- Validation (1)
- Vanadium redox flow battery (1)
- WAXS (1)
- Wastewater (1)
- Water samples (1)
- Welding (1)
- X-Ray Fluorescence (1)
- X-ray absorption spectroscopy (1)
- X-ray and electron diffraction (1)
- X-ray fluorescence spectroscopy (1)
- X-ray photoelectron spectroscopy (1)
- X-ray scattering (1)
- X-ray spectroscopy (1)
- XAS (1)
- Xerogel (1)
- Zearalenone (1)
- Zinc analysis (1)
- Zirconium (1)
- electrocatalysis (1)
- microplastics, sampling, sampling techniques, water (1)
- nanostructured (1)
- µJ-DPSS laser (1)
- Ägyptisches Museum Berlin (1)
Organisationseinheit der BAM
- 6 Materialchemie (197) (entfernen)
Paper des Monats
- ja (1)
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_1 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.
Mikroplastik Detektion mit Thermoanalytischen Methoden: Analytik, Referenzmaterial, Ringversuche
(2024)
Ich dem Vortrag geht es um die Vorstellung von thermoanalytischen Methoden für die Mikroplastik-Detektion. Verschiedene Kopplungsmöglichkeiten werden gezeigt und die Funktionsweise der TED-GC/MS wird erklärt. Im zweiten Teil werden Referenzmaterialien für die Mikroplastik-Analytik diskutiert. PET -Tabletten des PlasticTrace Projektes werden vorgestellt. Am Ende wird der VAMAS Ringversuch zur Mikroplastik-Detektion gezeigt.
This report contains detailed information on the preparation of the reference material as well as on homogeneity and stability investigations of the property of interest, the equivalent particle diameter, and on the analytical methods to determine the additional properties. The values for particle size distribution are based on the results from laser diffraction measurements of 3 different devices with at least 3 replicate measurements of 4 randomly chosen units of the reference material P206.
The talk summarizes challenges in microplastic analysis. It shows the preparation of microplastic reference materials as well as the testing on homogeneity and stability. The reference material is used in an international laboratory comparison to compare different detection methods used for microplastic analysis. The methods used were µ-IR (FTIR+LDIR) for number-based methods and TED-GC/MS and Py-GC/MS for mass-based methods. The ILC was done under the umbrella of VAMAS TWA 45. Results of the participants are presented.
Preliminary results of an interlaboratory comparison on microplastics organised by plasticsfate
(2023)
Microplastics are everywhere in the environment, but analytics is challenging. Since harmonisation is missing as well es suitable reference materials, BAM did under th umbrella of VAMAS funded by the EU Horizon 2020 project PlasticsFate a ILC for microplastic detection methods. Methods adressed were IR, Raman, Py-GC/MS and TED-GC/MS. The talk gives a first presentation and evaluation on the results.
Die Probenpräparation ist ein wichtiger Schritt für die Qualität der Massenspektren in MALDI-TOF MS. Es werden Polymerproben, die lösungsmittelbasiert und lösungsmittelfrei präpariert worden sind, verglichen. Dabei werden die Intensitätsverhältnisse von ternären Mischungen von PEG-, PS- und PMMA-Polymeren beachtet.
The presentation gives an overview of BAM's activities on processing influences and application properties of MPEAs in the form of joined and machined high and medium entropy alloys (CoCrFeMnNi and CoCrNi). In the case of welding, the focus is on defect-free welded joints with sufficient mechanical properties. In the case of machining, the focus is on the possible influence on the surface quality of the materials through adequate milling parameters. In addition, the hydrogen absorption and diffusion properties as well as the electrochemical corrosion behavior are fundamentally examined.
Solvent-free sample preparation offers some advantages over solvent-based techniques, such as improved accuracy, reproducibility and sensitivity, for matrix-assisted laser desorption/ionization (MALDI) analysis. However, little or no information is available on the application of solvent-free techniques for the MALDI analysis of polymer blends. Solvent-free sample preparation by ball milling was applied with varying sample-to-matrix ratios for MALDI time-of-flight mass spectrometry analysis of various polymers, including polystyrenes, poly(methyl methacrylate)s and poly(ethylene glycol)s. The peak intensity ratios were compared with those obtained after using the conventional dried droplet sample preparation method. In addition, solvent-assisted milling was also applied to improve sample homogeneities.
Depending on the sample preparation method used, different peak intensity ratios were found, showing varying degrees of suppression of the signal intensities of higher mass polymers. Ball milling for up to 30 min was required to achieve constant intensity ratios indicating homogeneous mixtures. The use of wet-assisted grinding to improve the homogeneity of the blends was found to be disadvantageous as it caused partial degradation and mass-dependent segregation of the polymers in the vials.The results clearly show that solvent-free sample preparation must be carefully considered when applied to synthetic polymer blends, as it may cause additional problems with regard to homogeneity and stability of the blends.
This is a set of use examples for the HDF5Translator framework. This framework lets you translate measurement files into a different (e.g. NeXus-compatible) structure, with some optional checks and conversions on the way. For an in-depth look at what it does, there is a blog post here.
The use examples provided herein are each accompanied by the measurement data necessary to test and replicate the conversion. The README.md files in each example show the steps necessary to do the conversion for each.
We encourage those who have used or adapted one or more of these exampes to create their own conversion, to get in touch with us so we may add your example to the set.
A poly(L-lactide) with a trifluoroethyl ester end group and an average degree of polymerization (DP) of 50 was synthesized by ROP of L-lactide initiated with trifluoroethanol. Small-angle X-ray scattering (SAXS) in combination with differential scanning calorimetry (DSC) measurements revealed an average crystal thickness of 13 nm, corresponding to 45 repeat units. This suggests that most crystallites were formed by extended PLA chains, and both flat surfaces were covered by CF3 groups. The crystalline PLAs were annealed at 140 or 160 °C in the presence of two catalysts: tin(II) 2-ethylhexanoate, (SnOct2) or dibutyltin bis(pentafluorophenoxide) (BuSnPhF). The chemical reactions, such as polycondensation and cyclization, proceeded in the solid state and were monitored by matrix-assisted laser desorption/ionization time-offlight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC) measurements. Under optimal conditions a large fraction of linear chains was transformed into crystallites composed of extended cycles. Additionally, MALDI TOF MS analysis of GPC fractions from samples annealed for 28 or 42 days detected chain elongation of the linear species up to a factor of 20.
Trinamic TMCL IOC is a Python package designed for controlling stepper motors connected to a Trinamic board using the TMCL language (all boards supported by PyTrinamic should now work, has been tested on the TMCM 6110 and the TMCM 6214). Since it is implementing the TMCL protocol, it should be easy to adapt to other Trinamic motor controller boards. This package assumes the motor controller is connected over a machine network via a network-to-serial converter, but the underlying PyTrinamic package allows for other connections too.
This allows the control of attached motors via the EPICS Channel-Access virtual communications bus. If EPICS is not desired, plain Pythonic control via motion_control should also be possible. An example for this will be provided in the example.ipynb Jupyter notebook.
This package leverages Caproto for EPICS IOCs and a modified PyTrinamic library for the motor board control, and interfaces between the two via an internal set of dataclasses. Configuration for the motors and boards are loaded from YAML files (see tests/testdata/example_config.yaml).
The modifications to PyTrinamic involved extending their library with a socket interface. This was a minor modification that should eventually find its way into the official package (a pull request has been submitted).
This presentation highlights ongoing scientific misconduct as found in academic literature. This includes data- and image manipulation, and paper mills. Starting with an expose of examples, it delves deeper into the causes and metrics driving this phenomenon. Finally a range of possible tools is presented, that the young researcher can use to prevent themselves from sliding into the dark scientific methods.
By automatically recording as much information as possible in automated laboratory setups, reproducibility and traceability of experiments are vastly improved. This presentation shows what such an approach means for the quality of experiments in an X-ray scattering laboratory and an automated synthesis set-up.
The principles of (Hard) X-ray photoelectron spectroscopy and some application in the field of (core-shell) nanoparticles will be presented. The presentation should answer hoe to get reliable results. Furthermore, examples of the correlation between physical-chemical measurments and toxicological results are given which are crucial for the risk assessment of nanoparticles.
The usefulness of seven different Tin catalysts, Bismuth subsalicylate and Titan tetra(ethoxide) for the polycondensation of ethyl L-lactate (ELA) was examined at 150 °C/6 d. Dibutyltin bis(phenoxides) proved to be particularly effective. Despite the low reactivity of ELA, weight average molecular masses (Mw) up to 12 500 were found along with partial crystallization. Furthermore, polylactides (PLAs) of similar molecular masses were prepared via ELA-initiated ROPs of L-lactide by means of the four most effective polycondensation catalysts. The crystalline linear PLAs were annealed at 140 or 160 °C in the presence of these catalysts. The consequences of the transesterification reactions in the solid PLAs were studied by means of matrix-assisted laser desorption/ionization (MALDI TOF) mass spectrometry, gel permeation chromatography (GPC) and small-angle X-ray scattering (SAXS). The results indicate that polycondensation and formation of cycles proceed in the solid state via formation of loops on the surface of the crystallites. In summary, five different transesterification reactions are required to explain all results.
Inputs of plastic impurities into the environment via the application of fertilizers are regulated in Germany and the EU by means of ordinances. Robust and fast analytical methods are the basis of legal regulations. Currently, only macro- and large microplastic contents (>1 mm) are measured. Microplastics (1–1,000 µm), are not yet monitored. Thermal analytical methods are suitable for this purpose, which can determine the mass content and can also be operated fully automatically in routine mode. Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) allows the identification of polymers and the determination of mass contents in solid samples from natural environments. In accordance with the German or European Commission (EC) Fertiliser Ordinance, composting plants should be monitored for microplastic particles with this method in the future. In this context a compost plant was sampled. At the end of the rotting process, the compost was sieved and separated in a coarse (>1 mm) and a fine fraction (<1 mm). The fine fraction was processed using density separation comparing NaCl and NaI as possible salt alternative and screened for microplastic masses by TED-GC/MS with additional validation and quality assurance experiments. With TED-GC/MS total microplastics mass contents of 1.1–3.0 μg/mg in finished compost could be detected with polyethylene mainly. What differs much to the total mass of plastics in the coarse fraction with up to 60 μg/mg, which were visually searched, identified via ATR-FTIR and gravimetrically weighted.
This contribution provides an overview of the BAMline synchrotron radiation beamline, which specializes in hard X-ray spectroscopy techniques for materials research. The BAMline offers X-ray absorption spectroscopy (XAS), x-ray fluorescence spectroscopy (XRF), and tomography to study materials' electronic structure, chemical composition, and structure. Key capabilities include standard and dispersive XAS for electronic structure, micro-XRF for elemental mapping, coded aperture imaging, and depth-resolved grazing exit XAS. The BAMline enables in situ characterization during materials synthesis and functions for energy, catalysis, corrosion, biology, and cultural heritage applications.
Ongoing developments like the implementation of machine learning techniques for experiment optimization and data analysis will be discussed. For instance, Bayesian optimization is being used to improve beamline alignment and scanning. An outlook to the future, where the BAMline will continue pioneering dynamic and multi-scale characterization, aided by advanced data science methods, to provide unique insights into materials research, will be given.
The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail.
Enhancing efficiency at bamline: employing data science and machine learning for x-ray research
(2023)
This talk discusses how data science and machine learning techniques are being applied at the BAM Federal Institute for Materials Research and Testing to enhance efficiency and automation at the BAMLine synchrotron facility. The methods presented include Gaussian processes and Bayesian optimization for beamline adjustment and optimization of X-ray measurements. These statistical techniques allow automated alignment of beamline components and active learning scanning to reduce measurement time.
Additional machine learning methods covered are neural networks for quantification of X-ray fluorescence (XRF) data and decoding coded apertures.
Mechanochemistry provides polymorphs that are difficult to obtain by conventional solution-based methods. Based on the nicotinamide and pimelic acid cocrystal, we demonstrated that the ball size, frequency, and temperature are essential parameters. Our results indicate that fine-tuning the energy input during a mechanochemical reaction can provide control over polymorphism.
Quantitative Analysis and 2D/3D Elemental Imaging of Cocoa Beans Using X‑ray Fluorescence Techniques
(2023)
As an important raw material for the confectionery industry, the cocoa bean (Theobroma cacao L.) has to meet certain legal requirements in terms of food safety and maximum contaminant levels in order to enter the cocoa market. Understanding the enrichment and distribution of essential minerals but also toxic metals is of utmost importance for improving the nutritional quality of this economically important raw food material. We present three X-ray fluorescence (XRF) techniques for elemental bio-imaging of intact cocoa beans and one additional XRF technique for quantitative analysis of cocoa pellets. The interrelation of all the methods presented gives a detailed picture of the content and 3D-resolved distribution of elements in complete cocoa beans for the first time.
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.
Im Verbundprojekt RUSEKU wurde die Probenahme von Wasserproben entscheidend weiterentwickelt. Wichtig ist hierbei zu gewährleisten, dass genügend Merkmalsträger in jeder Probe untersucht werden. Es muss daher eine für den Probenahmeort repräsentative Beprobung hinsichtlich des Wasservolumens in Abhängigkeit der Partikelanzahl gewährleistet sein.
Das Hauptaugenmerk lag im vorliegenden Projekt auf einer praxisnahen Beprobungsstrategie. Es wurden verschiedene Konzepte ausprobiert.
• Grundsätzlich hat sich gezeigt, dass eine Stichprobe eine Momentaufnahme des MP-Massengehaltes zeigt. Es wird eine hohe Statistik, also eine Vielzahl an Messungen am gleichen Probenahmeort, benötigt, um eine valide Aussage über den MP-Gehalt zu machen.
• Es zeigt sich, dass eine integrale Probenahme über mehrere Wochen mit dem SK routinemäßig möglich ist. Die erfassten MP-Massen sind reproduzierbar und robust.
• Die DFZ ist für Stichproben geeignet. Partikel < 50 µm werden eventuell unterschätzt
• Die fraktionierte Filtration kann für Stich- und Mischproben direkt im Feld genutzt werden. Fraktionen von 10 und 5 µm werden später im Labor Vakuum filtriert. Es erfolgt eine Fraktionierung der Probe mit Siebmaschenweiten von 1000, 500, 100, 50, 10 und 5 µm.
• Die fraktionierte Filtration kann auch anschließend an die Beprobung mit dem SK zur Anwendung kommen. Wird die mit dem SK gewonnene Wasserprobe fraktioniert filtriert, kann neben einem MP-Gesamtgehalt auch eine Einschätzung über die Partikelgrößen gewonnen werden.
• Für Wässer mit geringen Partikelzahlen wurde ein Messfiltertiegel entwickelt. Dieser hat eine Maschenweite von 6 µm. Seine Anwendung kann mögliche Verluste beim Transferieren vom Probenahmetool zum Messgefäß und mögliche Kontaminationen reduzieren.
Die Optimierung der Probenahmestrategie wurde durch Modellversuche und Simulationen unterstützt. Modellversuche zum Sinkverhalten und Simulationen von MP in realen Gewässern verdeutlichten das komplexe Verhalten der Partikel. Es konnte gezeigt werden, dass Partikel ab einer bestimmten Größe (und kleiner) bei genügend starker Turbulenz sich in der Wassersäule unabhängig von ihrer Dichte verhalten und so auch MP mit kleiner Dichte (z.B. PE) in der gesamten Wassersäule zu finden sind. Es konnte mit dem TEM die Existenz von NP gezeigt werden.
Ein wesentlicher Aspekt des RUSEKU Projektes war die Beprobung realer Kompartimente. Beprobt wurde neben Oberflächengewässern, das urbane Abwassersystem der Stadt Kaiserslautern, Waschmaschinenabwasser und Flaschenwasser.
• In Oberflächengewässern wurde hauptsächlich PE gefunden. Je nach Probe und Gewässer konnten auch PP, PS, PET, PA, SBR und Acrylate nachgewiesen werden.
• Im urbanen Abwassersystem der Stadt Kaiserslautern konnte an allen Probenahmestandorten MP nachgewiesen werden. Es wurde hauptsächlich PE, neben geringeren Mengen an PP, PS und SBR gefunden. Nach einem Regenereignis war der SBR Anteil deutlich erhöht.
• Die Beprobung eines realen Wäschepostens, bestehend aus T-Shirts und Hemden mit PA/CO oder PES/CO Mischgewebe, zeigte einen PA- und PES-Austrag im Waschwasser. Der überwiegende Teil der detektierten Fasern ist aber auf Baumwolle zurückzuführen. Reine gravimetrische Messungen zur Detektion von MP führen zu einer starken Überschätzung.
• In Flaschenwasser (PET-Flaschen) konnte MP detektiert werden. PET wurde nur im stillen Mineralwasser, nicht in Mineralwasser mit Kohlensäure gefunden werden. Teilweise wurde auch das MP-Material des Verschlusses im Wasser detektiert.
• Für Luftproben konnte ein Aufbau zur größenselektiven Beprobung getestet werden.
Neben der Probenahme hat das Projekt auch gezeigt, dass die TED-GC/MS geeignet für die MP-Detektion im Routinebetrieb ist. Die TED-GC/MS konnte weiter optimiert werden. Es wurden MP-Massen bestimmt.
Im Projekt wurden erste realitätsnahe Referenzmaterialien für die MP Detektion hergestellt. Die Herstellung von realitätsnahen Polymeren in ausreichender Homogenität und Menge hat sich als große Herausforderung herausgestellt.
Cardiac troponin I (cTnI) is a crucial biomarker for diagnosing cardiac vascular diseases, including acute myocardial infarction (AMI). This study presents a proof-of-concept chemiluminescence-based immunosensor for rapid and accurate measurement of cTnI, with the potential for online monitoring. The immunosensor incorporates a flow cell design and a sensitive complementary metal-oxide-semiconductor (CMOS) camera for optical readout. A microfluidic setup was established to enable selective and quasi-online determination of cTnI within ten minutes. The sensor was tested with recombinant cTnI in phosphate buffer, demonstrating measurements in the concentration range of 2–25 µg/L, with a limit of detection (LoD) of 0.6 µg/L (23 pmol/L) achieved using the optimized system. The immunosensor exhibited high selectivity, as no cross-reactivity was observed with other recombinant proteins such as cTnT and cTnC at a concentration of 16 µg/L. Measurements with diluted blood plasma and serum yielded an LoD of 60 µg/L (2.4 nmol/L) and 70 µg/L (2.9 nmol/L), respectively. This biosensor offers a promising approach for the rapid and sensitive detection of cTnI, contributing to the diagnosis and management of acute myocardial infarction and other cardiac vascular diseases.
Im der Präsentation werden, neben der Möglichkeit der Mikroplastikquantifizierung, auf weitere Anwendungsfelder der Methode TED-GC/MS eigegangen. Dies beinhaltet die Erfassung von Degradationsprodukten UV/O2 geschädigter Polymere und die Detektion von Additiven. Die Optimierung der Methode betreffend Messzeit und materialspezifischer Messanforderung sind ebenfalls Gegenstand.
Introduction to microplastics, definition, relevance, analytical approaches & challenges. TED-GC/MS working principle, features & performance. Optimisation in TED-GC/MS methodology, new validation data. Replacement of Internal Standard, outlook towards upcoming publication and application within EU´s revised drinking water directive.
This article describes the elaboration and characterization of diethylphosphonate-containing polymers coated electrodes as sensors for the detection of heavy metalstraces, by electrochemical impedance spectroscopy. Diethylphosphonate groupswere chosen as heavy metals binding sites. Two different series of polymers bearingthese anchoring groups were synthesized. Whereas the diethylphosphonate groupsare directly incorporated in the aromatic macromolecular chain in some polymers, analiphatic spacer is removing the chelating site from the polymer backbone in others.The influence of the macromolecular structure on the sensing response was studied,especially for the detection of Pb2+,Ni2+,Cd2+and Hg2+. Polymer P6, including thehigher amount of diethylphosphonate groups removed from the polymer chain by ashort alkyl spacer gave the higher sensitivity of detection of lead ions, with a detec-tion limit of 50 pM
Thermo-Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to investigate the thermal degradation of two different polyurethanes (PU). PU samples were heated at different heating rates and the desorbed products were collected in a cold injection system and thereafter submitted to GC-MS. Prospects and limitations of the detection and quantification of semi-volatile degradation products were investigated. A temperature dependent PU depolymerization was
found at temperatures above 200 °C proved by an increasing release of 1,4-butanediol and methylene diphenyl diisocyanate (MDI) representing the main building blocks of both polymers. Their release was monitored quantitatively based on external calibration with authentic compounds. Size Exclusion Chromatography (SEC) of the residues obtained after thermodesorption confirmed the initial competitive degradation mechanism indicating an equilibrium of crosslinking and depolymerization as previously suggested. Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry of SEC fractions of thermally degraded PUs provided additional hints on degradation mechanism.
To gain insight into the possible origin of the gold used in the production of tesserae containing gold leaf less than 0.5 μm thick placed between two layers of glass, we propose a non-destructive synchrotron radiation (SR) XRF protocol based on sequential analysis under optimised analytical conditions. Using this protocol, trace element analysis is achieved with detection limits of 1–6 mg/kg. As Pt and Au have adjacent fluorescence energies, we tested the most challenging situation, when Pt is present in very low concentrations in gold. Data obtained by double-dispersive XRF (D2XRF) and μXRF for fourth–ninth-century mosaics decorating nine Eastern and Western religious buildings show that the Eastern and Western tesserae are made from different alloys.
However, these alloys are identical to those used to make gold leaf for gilding, because plastic deformation requires the use of gold alloys with high ductility and malleability. Although trace element composition of gold used in the concerned period is only available for coins, by comparing the amounts of Pt contained in the tesserae and in the coins we show that Roman tesserae are made from Roman gold, as described in the documentary sources. We observe for the Byzantine period the use of a Byzantine gold and of gold supposedly from different stages of recycling, and we suggest the use of Umayyad and Abbasid gold for the production of Islamic tesserae.
In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other.
With the online coupling (or hyphenation) of chemically-resolved spectroscopy detection with classical size-exclusion chromatography (SEC) it is possible to correlate polymer molecular size with chemical structure in a single in-situ or on-flow measurement. Medium-resolution 1H-NMR (60 MHz) spectroscopy (i.e., “desktop NMR”) and Fouriertransform Infrared Spectroscopy (FTIR) have both been developed as coupled methods (SEC-MR-NMR, SEC-FTIR) for the detection of polymer analytes by monitoring e.g. alkene or carbonyl functionality.1,2 Here, we have investigated the potential for the detection of polymer end groups, using a slightly higher field-strength spectrometer (80 MHz 1H Larmor frequency) and taking advantage of a columnless injection method that provides bulk spectra for reference. End-functionalized polymers were synthesized by reaction of PEG with toluene isocyanate, yielding ,-functionalized polymers with exactly 2 IR- and NMR-detectable functional groups per chain, as proven by MALD-TOF mass spectrometry. We have investigated the sensitivity (limit of detection) and spectral resolution for these functional groups in chloroform, THF, and water. Results have demonstrated a good feasibility for the simultaneous online detection of PEG backbone (M~4000 g/mol) and these end groups at the level of ca. 2 mol%.
X-ray fluorescence imaging is a well-established tool in materials characterization. In this work, we present the adaption of coded aperture imaging to full-field X-ray fluorescence imaging at the synchrotron. Coded aperture imaging has its origins in astrophysics, and has several advantages: Coded apertures are relatively easy to fabricate, achromatic, allow a high photon throughput, and high angular acceptance. Coded aperture imaging is a two-step-process, consisting of the measurement process and a reconstruction step. Different programs have been written, for the raytracing/forward projection and the reconstruction. Experiments with coded aperture in combination with a Color X-ray Camera and an energy-dispersive area detector, have been conducted at the BAMline. Measured samples were successfully reconstructed, and gave a 9.1-fold increase in count rate compared to a polycapillary optic.
Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energydispersive array detector with a coded aperture to obtain high resolut ion images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @BESSY II. This method enables the simultaneous detection of multiple elements,which is important e.g. in the field of catalysis.
Detektion von Mikroplastik
(2022)
Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline
(2022)
For more than 20 years, BAM is operating the BAMline at the synchrotron BESSY II in Berlin Adlershof. During this time, the complexity of the setup and the amount of data generated have multiplied. To increase the effectiveness and in preparation for BESSY III, algorithms from the field of machine learning are increasingly used.
After a short introduction to BO and GP, the first example is the automatic alignment of our double multilayer monochromator (DMM).
The second example is the optimization of measurement time in XRF scanning.
News from the BAMline
(2022)
In this talk an overview about artificial intelligence/machine learning applications @BAMline is given. In the first part, the use of neural networks for the quantification of XRF measurements and the decoding of coded-aperture measurements are shown. Then it is shown how Gaussian processes and Bayesian statistics can be used to achieve an optimal alignment of the set-up and in general for optimization of measurements.
Gold is one of the seven metals already known in antiquity and was used from time immemorial as a medium of exchange and for the production of jewelry because of its luster and rarity. In addition, it is easy to work and largely resistant to chemical influences. Investigations of gold using synchrotron radiation excited X-ray fluorescence analysis are non-destructive and provide information about the chemical elements present in the sample under investigation. The investigations presented here at BAMline focus on questions such as the origin, manufacturing process, and association of gold findings. The different questions are explained by a number of examples ranging from the Viking treasure from Hiddensee to the Nebra Sky Disk and finds from Egypt. The find from Bernstorf is discussed in detail. A Bayesian treatment of the authenticity is shown.
n this study, two green synthesis routes were used for the synthesis of Ag/ZnO nanoparticles, using cassava starch as a simple and low-cost effective fuel and Aloe vera as a reducing and stabilizing agent. The Ag/ZnO nanoparticles were characterized and used for bacterial dis-
infection of lake water contaminated with Escherichia coli (E. coli). Characterization indicated the formation of a face-centered cubic structure of metallic silver nanoparticles with no insertion of Ag into the ZnO hexagonal wurtzite structure. Physicochemical and bacteriological analyses described in “Standard Methods for the Examination of Water and Wastewater” were used to evaluate the efficiency of the treatment. In comparison to pure ZnO, the synthesized Ag/ZnO nanoparticles showed high efficiencies against Escherichia coli (E. coli) and general coliforms present in the lake
water. These pathogens were absent after treatment using Ag/ZnO nanoparticles. The results indicate that Ag/ZnO nanoparticles synthesized via green chemistry are a promising candidate for the treatment of wastewaters contaminated by bacteria, due to their facile preparation, low-cost synthesis,and disinfection efficiency.
Microplastic detection in water samples becomes important for tracing microplastic sources. Microplastic may harm desalination facilities by blocking filters and disturbing the marine food chain. Thermo analytical methods such as pyrolysis gas chromatography mass spectroscopy, and spectroscopic methods like (micro) Raman spectroscopy or (micro) Fouriertransform infrared spectroscopy in combination with appropriate filters and sample preparation are suitable for analyzing microplastics on a scale from 1 µm to 1000 µm fast and unambiguous. While the thermo analytical methods are suitable for larger sample volumes, Raman spectroscopy and Fouriertransform infrared spectroscopy are able to detect and analyze single microplastic particles for instance in bottled water. Machine learning algorithms ensure a reliable classification of different plastic materials.
Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine (TMB) in Amperometric Assays
(2022)
Electrochemical methods make great promise to meet the demand for user-friendly on-site devices for monitoring important parameters. Food industry often runs own lab procedures, e.g. for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with miniaturized technologies. Enzyme-linked immunosorbent assays, with photometric detection of the horseradish peroxidase (HRP) substrate, 3,3’,5,5’-tetramethylbenzidine (TMB), form a good basis for sensitive detection. To provide a straight-forward approach for the miniaturization of the detection step, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry it was found that the TMB electrochemistry is strongly dependent on the pH and the electrode material.
It was found that screen-printed gold electrodes and a highly acidic pH value (pH 1) are well-suited to perform the electrochemical detection of TMB, due to the reversible character of the redox reaction under these conditions. This set-up provides a good signal stability over several measuring cycles, providing the basis for analysing multiple samples. In contrast to this, for carbon screen-printed electrodes, it was found that the signal response has changed after the electrochemical reaction with TMB at pH 1. At a weakly acidic pH value (pH 4), neither with carbon nor with gold electrodes a reproducible electrochemical detection of TMB could be achieved [1].
Based on these findings we created a smartphone-based, electrochemical, immunomagnetic assay for the detection of ochratoxin A and ergometrine in real samples. Therefore, a competitive assay was performed on magnetic beads using HRP and TMB/H2O2 to generate the signal. Enzymatically oxidized TMB was quantified after addition of H2SO4 by amperometry with screen-printed gold electrodes in a custom-made wall-jet flow cell. The results are in good correlation with the established photometric detection method, providing a solid basis for sensing of further analytes in HRP-based assays using the newly developed miniaturized smartphone-based, electrochemical, immunomagnetic assay.
Soil acts as a final sink for pollutants. Microplastics from different sources such as plastic mulching, littering, compost, sewage sludge, sedimentary deposition, and tyre abrasion are expected to be found in soil. However, representative and comprehensive information is missing on the sources, transport, and fate. Therefore, a reliable analysis method for microplastics in soils needs to be developed.
The presented work describes the development of a procedure for microplastics analysis in soils. A representative sampling based on the on-site conditions and a sample preparation method was established and comprised of a drying step, the separation of microplastic particles > 1 mm, and a density separation for particles < 1 mm. The detection of the large microplastic particles (> 1 mm) was conducted with Attenuated Total Reflection - Fourier Transform infrared Spectroscopy (ATR-FTIR) , while Thermal Extraction Desorption - Gas Chromatography / Mass Spectrometry (TED-GC/MS) was applied for particles < 1 mm, gaining information on the type of polymer and mass fraction. Based on the established method, 14 environmental soil samples ? with different exposure of microplastics from agriculture, industrial sites, roads, and floods were investigated.
Due to the arbitrary microplastic particle distribution among the samples for large microplastics, it was reasoned that the found particles were unrepresentative. In contrast, microplastic particles < 1 mm were discovered in a high mass in soil samples exposed to plastic mulching or fertilization with sewage sludge or compost (0 – 115 mg/kg). On average, microplastic contents detected in soil samples taken from a construction site and an inner-city lake were higher (13 – 238 mg/kg). As expected, microplastic content in soil sampled in proximity to roads was more pronounced in the upper soil layers. In contrast, very remote sampling sites, expectably uncontaminated, did not lead to the detection of microplastic regarding to thermoanalytical detection method.
In a proof of concept experiment several in vivo and in vitro ecotoxicological tests were applied to evaluate the effect of microplastics (tyre abrasion, polystyrene containing hexabromocyclododecane) in natural soils. In summary, while no effects of the examined probes could be detected on higher levels of biological organization after exposures to earthworm E. andrei, significant changes in several oxidative stress related biomarkers were observed.
Measuring an X-ray scattering pattern is relatively easy, but measuring a steady stream of high-quality, useful patterns requires significant effort and good laboratory organization.
Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration).
With the MOUSE, we have combined a comprehensive and highly automated laboratory workflow with a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data.
This talk will briefly introduce the foundations of X-ray scattering, present the MOUSE project, and will highlight the proven utility of the methodology for materials science. Upgrades to the methodology will also be discussed, as well as possible avenues for transferring this holistic methodology to other instruments
Li-rich nanoparticles of Li1+xMn2–xO4 doped with Al, Co, or Ni are successfully synthesized using a facile, fast, and efficient microwave-assisted hydrothermal route. Synchrotron X-ray diffraction confirms the formation of the crystalline cubic spinel phase type. X-ray absorption spectroscopy analysis at the Co and Ni K- and L-edges verifies that the dopants are within the Li1+xMn2–xO4 spinel structure and are inactive during cycling in the bulk and at the surface. Moreover, we demonstrate that nanocrystallinity and cationic doping play an important role in improving the electrochemical performance with respect to LiMn2O4 microparticles. They significantly reduce the charge-transfer resistance, lower the first cycle irreversible capacity loss to 6%, and achieve a capacity retention between 85 and 90% after 380 cycles, with excellent Coulombic efficiency close to 99% without compromising the specific charge at a 5C cycling rate. Furthermore, the Mn K- and L-edges attest that after long cycling, the Mn oxidation state in the bulk differs from that at the surface caused by the Mn disproportion reaction; however, the cationic doping helps mitigate the Mn dissolution with respect to the undoped Li1+xMn2–xO4 nanoparticles, as indicated by inductively coupled plasma atomic emission spectrometry.