TY - CONF A1 - Alasonati, E A1 - Bartczak, D A1 - Altmann, Korinna A1 - Giovannozzi, A T1 - Towards Standardised Micro and Nanoplastics Analysis via Interlaboratory Comparisons: First Outlook of the VAMAS TWA 45 P3 Project N2 - This talk is part of the stakeholder workshop of the PlasticTrace project held in September 2025 in Oslo. The presentation shows first results of the VAMAS ILC on nanoplastics. PP nanoparticles were given to the participants. These were asked to measure the mass or particle number or size of the PP nanoplastics. Various techniques such as DLS, FFF, Py-GC/MS, TED-GC/MS, PTA were used. T2 - Stakeholder Workshop PlasticsTrace CY - Online meeting DA - 09.09.2025 KW - Nanoplastics KW - ILC KW - DLS KW - Polypropylene PY - 2025 AN - OPUS4-64714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grimmer, Christoph A1 - Richter, Matthias A1 - Neuhaus, T. A1 - Prinz, Carsten A1 - Strzelczyk, Rebecca Skadi A1 - Colakoglu, Irem A1 - Horn, Wolfgang T1 - Towards a multi-VOC emission reference material with temporally constant emission profile for QA/QC of materials emission testing procedures N2 - Emission reference materials (ERMs) are sought after to further control and improve indoor air quality. The impregnation of porous materials with volatile organic compounds (VOCs) is a promising approach to produce ERMs. Different VOCs were used to impregnate various porous materials (mainly zeolites, activated carbons and a metal organic framework). The influence of different methodological parameters and material properties were studied to optimize the impregnation procedure and to find the best material/VOC combination. The impregnation procedure remains quite irreproducible, nevertheless, very good ERM candidates were identified. Two materials (zeolite 4 and AC 1 impregnated with n-hexadecane) showed a very stable emission over 14 days (<10 % change). Another material (AC 1 impregnated with toluene) showed a declining emission profile but with a very good in-batch reproducibility and a storage stability of up to 12 months. KW - Emission reference material KW - Porous materials KW - Indoor air quality KW - Emission test chamber KW - CO2 assisted impregnation KW - EN 16516 PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612238 DO - https://doi.org/10.1016/j.chemosphere.2024.143437 SN - 1879-1298 VL - 366 SP - 1 EP - 8 PB - Elsevier AN - OPUS4-61223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lee, C. A1 - Inutan, E. D. A1 - Chen, J. L. A1 - Mukeku, M. M. A1 - Weidner, Steffen A1 - Trimpin, S. A1 - Ni, C.-K. T1 - Toward understanding the ionization mechanism of matrix‐assisted ionization using mass spectrometry experiment and theory N2 - Matrix‐assisted ionization (MAI) mass spectrometry does not require voltages, a laser beam, or added heat to initiate ionization, but it is strongly dependent on the choice of matrix and the vacuum conditions. High charge state distributions of nonvolatile analyte ions produced by MAI suggest that the ionization mechanism may be similar to that of electrospray ionization (ESI), but different from matrix‐assisted laser desorption/ionization (MALDI). While significant information is available for MAI using mass spectrometers operating at atmospheric and intermediate pressure, little is known about the mechanism at high vacuum. Eleven MAI matrices were studied on a high‐vacuum time‐of‐flight (TOF) mass spectrometer using a 266 nm pulsed laser beam under otherwise typical MALDI conditions. Detailed comparisons with the commonly used MALDI matrices and theoretical prediction were made for 3‐nitrobenzonitrile (3‐NBN), which is the only MAI matrix that works well in high vacuum when irradiated with a laser. Screening of MAI matrices with good absorption at 266 nm but with various degrees of volatility and laser energies suggests that volatility and absorption at the laser wavelength may be necessary, but not sufficient, criteria to explain the formation of multiply charged analyte ions. 3‐NBN produces intact, highly charged ions of nonvolatile analytes in high‐vacuum TOF with the use of a laser, demonstrating that ESI‐like ions can be produced in high vacuum. Theoretical calculations and mass spectra suggest that thermally induced proton transfer, which is the major ionization mechanism in MALDI, is not important with the 3‐NBN matrix at 266 nm laser wavelength. 3‐NBN:analyte crystal morphology is, however, important in ion generation in high vacuum. The 3‐NBN MAI matrix produces intact, highly charged ions of nonvolatile compounds in high‐vacuum TOF mass spectrometers with the aid of ablation and/or heating by laser irradiation, and shows a different ionization mechanism from that of typical MALDI matrices. KW - Ionization KW - MALDI-TOF MS KW - Mechanism PY - 2021 DO - https://doi.org/10.1002/rcm.8382 VL - 35 IS - 51 SP - e8382 PB - John Wiley & Sons AN - OPUS4-49209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Casali, C. A1 - Feiler, Torvid A1 - Heilmann, Maria A1 - Braga, D. A1 - Emmerling, Franziska A1 - Grepioni, F. T1 - Too much water? Not enough? In situ monitoring of the mechanochemical reaction of copper salts with dicyandiamide N2 - n situ monitoring of mechanochemical reactions between dicyandiamide (DCD) and CuX2 salts (X = Cl−, NO3−), for the preparation of compounds of agrochemical interest, showed the appearance of a number of phases. It is demonstrated that milling conditions, such as the amount of water added in wet grinding and/or the milling frequency, may affect the course of the mechanochemical reactions, and drive the reaction towards the formation of different products. It has been possible to discover by in situ monitored experiments two novel crystalline forms, namely the neutral complexes [Cu(DCD)2(OH2)2(NO3)2] (2) and [Cu(DCD)2(OH2)Cl2]·H2O (4), in addition to the previously known molecular salt [Cu(DCD)2(OH2)2][NO3]2·2H2O (1, DIVWAG) and neutral complex [Cu(DCD)2(OH2)Cl2] (3, AQCYCU), for which no synthesis conditions were available. Compounds 2 and 4 were fully characterized via a combination of solid-state techniques, including X-ray diffraction, Raman spectroscopy and TGA. KW - Mechanochemistry KW - In situ PY - 2022 DO - https://doi.org/10.1039/d1ce01670a VL - 24 IS - 6 SP - 1292 EP - 1298 PB - RSC AN - OPUS4-54344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, U. T1 - Thermoanalytical methods to measure mass in microplastics N2 - The talk adresses the use of thermoanalytical methods in microplastics analysis. T2 - EUROLAB webinar: MICROPLASTICS: regulations, standards and the role of laboratories CY - Online meeting DA - 15.02.2023 KW - TED-GC/MS KW - Thermoanalytical methods KW - Microplastic mass PY - 2023 AN - OPUS4-57009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Scholz, Philipp A1 - Jung, Christian A1 - Weidner, Steffen T1 - Thermo-Desorption Gas Chromatography-Mass Spectrometry for investigating the thermal degradation of polyurethanes N2 - 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. KW - Thermo-desorption KW - Mass spectrometry KW - Polyurethanes KW - Thermal degradation PY - 2023 DO - https://doi.org/10.1039/D3AY00173C SN - 1759-9660 SP - 1 EP - 6 PB - Royal Society for Chemistry AN - OPUS4-57307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - The SMURFnano project - standardized measurements of surface functionalities on nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, optoelectronics, and information storage. NP function, interaction with biological species, and environmental fate are largely determined by surface functionalities. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Also, industry, international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required and well characterized test and reference nanomaterials providing benchmark values.[1] These needs are addressed by the recently started European metrology project SMURFnano involving 12 partners from different National Metrology Institutes, designated institutes, and research institutes, two university groups as well as one large company and one SME producing NPs. This project as well as first results derived from the development of test and reference materials with a well characterized surface chemistry and ongoing interlaboratory comparisons will be presented. T2 - eMRS CY - Strasbourg, France DA - 27.05.2025 KW - Quality assurance KW - Reference analysis KW - Standardization KW - Metrology KW - Reference products KW - Reference materials KW - Mission KW - Surface chemistry KW - Nano KW - Particle KW - qNMR KW - XPS KW - Fluorescence KW - Optical assays KW - Interlaboratory comparison KW - Uncertainty PY - 2025 AN - OPUS4-63243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - The emp project smurfnano – Standardizing the quantification of surface functionalities, ligands, and coatings on nanomaterials N2 - For industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage, meanwhile engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated. NP function, interaction with biological species, and environmental fate are largely determined by surface functionalities. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Also, industry, international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. These needs are addressed by the recently started European metrology project SMURFnano involving 12 partners from different National Metrology Institutes, designated institutes, and research institutes, two university groups as well as one large company and one SME producing NPs. This project as well as first results derived from the development of test and reference materials with a well characterized surface chemistry and ongoing interlaboratory comparisons will be presented. T2 - LNE Workshop CY - Paris, France DA - 04.11.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Characterization KW - Advanced material KW - Surface KW - Standardization KW - Reference material KW - Functional group KW - Quantification KW - Coating KW - Automation KW - Potentiometry KW - Method KW - Validation KW - Optical assay KW - Fluram KW - qNMR KW - Comparison KW - ILC PY - 2025 AN - OPUS4-64725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The Dark Side of Science (2024 edition) N2 - 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. T2 - Winter School on Metrology and Nanomaterials for Clean Energy CY - Claviere, Italy DA - 28.01.2024 KW - Scientific misconduct KW - Data manipulation KW - Image manipulation KW - Paper mills KW - Causes leading to scientific misconduct KW - Tools to combat scientific misconduct KW - Metrics PY - 2024 AN - OPUS4-59622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Textile Fibers as Reference Materials for Microplastic Release N2 - Fibers of textile origin are named as high contributor for microplastic pollution in the environment next to e.g. plastics from packaging, tire wear and paints. Small fibers and fragments (microplastics: 1-1000 µm) can be released from textiles by mechanical abrasion during application (e.g. wearing) or washing. To date, the occurrence, transport pathways, and impacts of such small fibers on the environment and human health remain unclear. The European Commission revised the Urban Wastewater Treatment Directive (Directive (EU) 2024/3019) and made monitoring of microplastics mandatory in the next years. Additionally, standards for microplastic detection are developed in the ISO standardization body ISO/TC 147/SC 2 with the documents ISO/DIS 16094-2 and ISO/DIS 16094-3. Detection mainly occurs by thermoanalytical methods for mass or vibrational methods with microscopes for numbers. Such standards and regulatory efforts need validated methods, which themselves need reference materials for validation. Reference materials are well characterized materials that are produced for a specific purpose and are homogeneous and stable within one property of interest. The shape and the composition of the reference particles/fibers will affect the detection, hence it is important to validate the instruments with fibers, if this is the task for monitoring campaigns. This work describes the production of realistic fibers as reference material for microplastic analysis. The individual samples contain of a small number (< 1000) and mass (< 20 µm) of fibres. Homogeneity and stability control occurred by thermogravimetric analysis and µ-Raman. Further characteristics were determined for type, shape and size distribution. T2 - TEXTEH CY - Bucharest, Romania DA - 23.10.2025 KW - Microplastics KW - Reference materials KW - Microfibers KW - Microfiber release PY - 2025 AN - OPUS4-64620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Synthesis of cyclic polymers and flaws of the Jacobson–Stockmayer theory N2 - Cyclic poly(L-lactide)s were prepared by ring-opening polymerization combined with simultaneous polycondensation (ROPPOC) in bulk at 160 ° with dibutyltin bis(4-cyanophenoxide) as catalyst. It is demonstrated by MALDI TOF mass spectrometry and 1H NMR end group analyses that cycles are formed by endto-end cyclization in addition to “back-biting” transesterification. Formation of high molar mass cyclic poly L-lactide)s by means of several more reactive ROPPOC catalysts presented previously and in new experiments is discussed. These experimental results, together with theoretical arguments, prove that part of the Jacobson–Stockmayer theory is wrong. The critical monomer concentration, above which end-toend cyclization is seemingly impossible, does not exist and reversible like irreversible polycondensations can theoretically proceed up to 100% conversion, so that finally all reaction products will necessarily adopt a cyclic architecture. KW - Polylactide KW - MALDI-TOF MS KW - Cyclization PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506419 DO - https://doi.org/10.1039/d0py00226g VL - 11 IS - 14 SP - 2595 EP - 2604 PB - Royal Society for Chemistry AN - OPUS4-50641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de O. Primo, J. A1 - Horsth, D.F. A1 - de S. Correa, J. A1 - Das, A. A1 - Bittencourt, C. A1 - Umek, P. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Yusenko, Kirill A1 - Zanetta, C. A1 - Anaissi, F.J. T1 - Synthesis and Characterization of Ag/ZnO Nanoparticles for Bacteria Disinfection in Water N2 - 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. KW - Synchrotron KW - BAMline PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562440 DO - https://doi.org/10.3390/nano12101764 SN - 2079-4991 VL - 12 IS - 10 SP - 1 EP - 18 PB - MDPI CY - Basel AN - OPUS4-56244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - Syntheses of cyclic polylactides and the problem of catenane formation N2 - Cyclic poly(L-lactide)s (PLAs) were prepared in bulk either by ring-expansion polymerization (REP) or by ring-opening polymerization (ROP) with simultaneous polycondensation (ROPPOC). In contrast to REP the latter method involves formation of linear chains and thus, may involve formation of polydisperse catenanes that affect crystallization. The reprecipitated PLAs were annealed at 120 °C and compared with regard to melting temperature (Tm) and melting enthalpy (ΔHm). For similar molar masses the PLAs prepared by REP and ROPPOC had almost identical Tm's and crystallinities. Furthermore, the influence of REP and ROPPOC catalysts on the morphology of the virgin reaction products was compared. KW - MALDI-TOF MS KW - Catenane KW - Polylactide PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625061 DO - https://doi.org/10.1039/d4ra08683j VL - 15 IS - 5 SP - 3686 EP - 3692 PB - RSC AN - OPUS4-62506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Drago, Claudia T1 - Sweetening the (microplastics) pill: PET tablets (1-100µm) as candidate reference material for the validation of microplastics measurement N2 - The lack of validation and standard procedures in microplastics studies has led to the inability to compare and harmonise data from different analytical methods, laboratories and time scales. To monitor and regulate exposure to microplastics in the environment and in food for human health, it is crucial to ensure their comparability and to validate the analytical methods used in microplastics studies. Monitoring microplastics requires complex approaches for accurate determination otherwise it can lead to an over- or underestimation in environmental and food-relevant matrices. Moreover, to support the need of reliable measurement required by the European legislation directive on drinking water (EU 2020/2184) or the revision of the urban waste water directive, which will be finalised in 2024 the production and validation of polymeric reference materials with environmentally relevant concentrations, irregular shapes, defined aging status and different sizes is essential. The production of reference material with acceptable uncertainties in homogeneity need to be balanced, considering the low microplastics concentrations detected in the environment and in food. The aim of the project PLASTICTRACE and of this study, is to propose a “easy-to-use PET tablet ” (PET particle size mainly 1-100 µm) for routine applications as a candidate general reference material for detection methods. Batches of water-soluble matrix containing different concentrations of PET powder were produced. Results of imaging and counting methods (SEM, Laser diffraction), including production´s challenges; together with thermo-analytical methods (TED-GC/MS and Py-GC/MS) and vibrational spectroscopy (µ-Raman and µ-FTIR), will be presented. These data are useful to assess homogeneity and stability of the particles over time according to ISO 33405:2024. In addition, we will show some insights on the application of the PET-tablets in complex matrices, as milk powder and suspended solid from surface water, that could be easily used for routine microplastics analysis. T2 - MICRO 2024 CY - Arrecife, Spain DA - 23.09.2024 KW - Microplastics KW - Reference materials KW - Polymer 3R KW - TED-GC/MS PY - 2024 AN - OPUS4-61274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine (TMB) in Amperometric Assays N2 - 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. T2 - Electrochemistry 2022 CY - Berlin, Germany DA - 28.09.2022 KW - Cylic Voltammetry KW - Immunoassay KW - TMB KW - Amperometry PY - 2022 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-55876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Andreas A1 - Weidner, Steffen A1 - Kricheldorf, Hans R. T1 - Star-shaped poly(l-lactide)s based on pentaerythritol: About crystallization and polycondensation plus disproportionation and ring formation in the solid state N2 - Star-shaped poly( L-lactide)s (s-PLAs), were prepared by ring-opening polymerization of with pentaerythritol and catalyzed by tin(II) 2-ethylhyexanoate (SnOct out in bulk at either 120 ◦ C or 160 ◦ L-lactide (LA) initiated 2 ). Two small series of ROPs were carried C with variation of the LA/initiator ratio. Matrix-assisted laser desorption/ ionization time-of-flight (MALDI-TOF) mass spectra revealed traces of cycles in 120 ◦ C samples only at low initiator/catalyst ratios. In contrast, higher fractions of cycles were detected in samples prepared at 160 C, suggesting a "back-biting" origin. The influence of arm length and thermal history on crystallinity was investigated by differential scanning calorimetry (DSC) and wide-angle x-ray scattering (WAXS). It was shown that annealing increased the melting temperature (T ◦ ◦ m ) and crystallinity. However, annealing at 140 ◦ C for 14 d also caused significant solid-state transesterification. In addition, crystallites composed of s-PLAs with extended arms and, simultaneously, crystallites composed exclusively of extended rings were formed, identified by their typical "sawtooth" pattern in the MALDI mass spectra. Small angle x-ray scattering (SAXS) indicated that the crystal thickness was lower than that of linear PLAs annealed under identical conditions, but increased upon annealing at 140 C. KW - MALDI-TOF MS KW - Polylactide KW - Crystallisation KW - AStar-shaped polymers PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636832 DO - https://doi.org/10.1016/j.polymer.2025.128709 SN - 0032-3861 VL - 334 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-63683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardized Measurements of Surface Functionalities on Nanoparticles - F. Synthesis and characterization of functional nanocomposite materials N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely and commonly fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage. NP function, their interaction with biological species, and also their environmental fate are largely determined by the surface functionalities of the particles. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, determination of their applicability, and mandatory to meet increasing concerns regarding their safety. In addition, industry as well as international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized up until now. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR), as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter, typically less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required to provide well characterized test and reference nanomaterials including benchmark values.[1] These needs are addressed by the current European metrology project SMURFnano, involving 12 partners from different National Metrology Institutes, designated and research institutes, two university groups as well as one large company and one SME producing NPs. This project, as well as first results derived from the development of test and reference materials with a well characterized surface chemistry, and ongoing interlaboratory comparisons, will be presented. T2 - Shift 2025 CY - La Laguna, Tenerife DA - 13.10.2025 KW - Nano KW - Particle KW - Silica KW - Iron oxide KW - Lanthanide KW - Metrology KW - Quality assurance KW - Reference material KW - Surface chemistry KW - Size KW - Shape KW - Particle number concentration KW - Method KW - Optical assay KW - qNMR KW - Validation KW - Potentiometry KW - XPS KW - ILC KW - Standardization PY - 2025 AN - OPUS4-64370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Standardized Measurements of Surface Functionalities on Nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely and commonly fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage. NP function, their interaction with biological species, and also their environmental fate are largely determined by the surface functionalities of the particles. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, determination of their applicability, and mandatory to meet increasing concerns regarding their safety. In addition, industry as well as international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized up until now. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR), as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter, typically less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required to provide well characterized test and reference nanomaterials including benchmark values.[1] These needs are addressed by the current European metrology project SMURFnano, involving 12 partners from different National Metrology Institutes, designated and research institutes, two university groups as well as one large company and one SME producing NPs. This project, as well as first results derived from the development of test and reference materials with a well characterized surface chemistry, and ongoing interlaboratory comparisons, will be presented. T2 - eMRS - Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Nano KW - Particle KW - Silica KW - Polymer KW - Metrology KW - Quality assurance KW - Reference material KW - Surface chemistry KW - Size KW - Shape KW - Particle number concentration KW - Method KW - Optical assay KW - qNMR KW - Validation KW - Potentiometry KW - XPS PY - 2025 AN - OPUS4-64243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardized Measurements of Surface - Functionalities on Nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, optoelectronics, and information storage. NP function, interaction with biological species, and environmental fate are largely determined by surface functionalities. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Also, industry, international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required and well characterized test and reference nanomaterials providing benchmark values.[1] These needs are addressed by the recently started European metrology project SMURFnano involving 12 partners from different National Metrology Institutes, designated institutes, and research institutes, two university groups as well as one large company and one SME producing NPs. This project as well as first results derived from the development of test and reference materials with a well characterized surface chemistry and ongoing interlaboratory comparisons will be presented. T2 - eMRS CY - Strasbourg, France DA - 27.05.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Silica KW - Upconversion nanoparticles KW - Optical assay KW - qNMR KW - Surface analysis KW - Ligand KW - Quantification KW - Functional group KW - XPS KW - ToF-SIMS KW - Polymer particle KW - Surface modification KW - Potentiometry KW - Metrology KW - Method KW - Validation KW - ILC PY - 2025 AN - OPUS4-63339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Giovannozzi, A T1 - Standardization and Harmonization Effort on Microplastics Analysis by Spectroscopic Methods N2 - This talk presents the EU funded project PlasticTrace. It shows the challenges in micro- and nanoplastic reference materials and gives some solutions regarding spectroscipc methods such as Raman or IR microscopy to determine the particle numbers. Materials are prepared by cryo milling to get some powder that is later pressed into tablets. The polymer type used is PET, because that is highly important for drinking water directive of EU commission. T2 - International Conference on Raman Spectroscopy (ICORS) CY - Roma, Italy DA - 28.07.2024 KW - Microplastics KW - Reference materials KW - Polymer 3R PY - 2024 AN - OPUS4-60881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Stakeholder Workshop – Plastictrace WP1 N2 - The talk is about WP1 in the PlasticTrace project funded by Euromat. The projects harmonizes microplastic analysis by developing SOPs and reference materials. WP1 is responsible for material selection and preparation. All particles are homogeneity and stability checked according to ISO guide 35. T2 - Stakeholder workshop of PlasticTrace project CY - Online meeting DA - 14.12.2022 KW - Microplastic KW - Microplastics standardisation KW - Reference materials PY - 2022 AN - OPUS4-56772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peters, Stefan A1 - Bartling, Stephan A1 - Parlinska-Wojtan, Magdalena A1 - Wotzka, Alexander A1 - de Oliveira Guilherme Buzanich, Ana A1 - Wohlrab, Sebastian A1 - Abdel-Mageed, Ali M. T1 - Stabilization of intermediate Mo oxidation states by Nb doping enhancing methane aromatization on Mo/HZSM-5 catalysts N2 - The dehydroaromatization of methane is a promising process to produce aromatics and ultra-pure hydrogen. Increased yields and stability of Mo/HZSM-5 against irreversible deactivation were achieved via a redox interaction by doping with otherwise inert Nb. KW - General Materials Science KW - Sustainability and the Environment KW - General Chemistry KW - Renewable Energy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597670 DO - https://doi.org/10.1039/D3TA07532J SN - 2050-7488 SP - 1 EP - 16 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - SRXRF examples from the BAMline N2 - Synchrotron radiation sources with their unique properties in terms of intensity, polarization and adjustability offer a wide range of possibilities in materials research. A basic introduction about the creation and special properties of synchrotron radiation will be given. Examples of current work at BAMline, the high-energy measuring facility of the Federal Institute for Materials Research and Testing at the synchrotron BESSY, are used to illustrate the possibilities and limitations of existing measuring methods. T2 - Better with Scattering CY - Online meeting DA - 16.03.2020 KW - Synchrotron KW - BAMline KW - XRF PY - 2020 AN - OPUS4-51895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dalgic, Mete-Sungur A1 - Weidner, Steffen T1 - Solvent-free sample preparation for matrix-assisted laserdesorption/ionization time-of-flight mass spectrometry ofpolymer blends N2 - 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. KW - MALDI TOF MS KW - Sample preparation KW - Polymer blends KW - Solvent-free PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598570 DO - https://doi.org/10.1002/rcm.9756 SN - 0951-4198 VL - 38 IS - 12 SP - 1 EP - 9 PB - Wiley online library AN - OPUS4-59857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Meyer, A. A1 - Falkenhagen, Jana A1 - Kricheldorf, H. R. T1 - SnOct2-catalyzed and alcohol-initiated ROPs of L-lactide – About the influence of initiators on chemical reactions in the melt and the solid state N2 - SnOct2 (Sn(II) 2-ethylhexanoate) catalyzed ROPs of L-lactide were performed in bulk with eight different alcohols as initiators. The time was varied between 1 h and 24 h for all initiators. For two initiators the temperature was also lowered to 115 ◦C. Even-numbered chains were predominantly formed in all polymerizations at short times, but the rate of transesterification (e.g. even/odd equilibration) and the molecular weight distribution were found to depend significantly on the nature of the initiator. Observed transesterification reactions also continued in solid poly (L-lactide), and with the most active initiator, almost total equilibration was achieved even at 130 ◦C. This means that all chains including those of the crystallites were involved in transesterification reactions proceeding across the flat surfaces of the crystallites. The more or less equilibrated crystalline polylactides were characterized by DSC and SAXS measurements with regard to their melting temperature (Tm), crystallinity and crystal thickness. KW - Polylactide KW - MALDI-TOF MS KW - Crystallization KW - Catalysts KW - SAXS PY - 2021 DO - https://doi.org/10.1016/j.eurpolymj.2021.110508 VL - 153 SP - 110508 PB - Elsevier Ltd. AN - OPUS4-52633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Braun, U. A1 - Herper, D. A1 - Knefel, M. A1 - Bednarz, M. A1 - Bannick, C.-G. T1 - Smart filters for the analysis of microplastic in beverages filled in plastic bottles N2 - The occurrence of microplastic (MP) in food products, such as beverages in plastic bottles, is of high public concern. Existing analytical methods focus on the determination of particle numbers, requiring elaborate sampling tools, laboratory infrastructure and generally time-consuming imaging detection methods. A comprehensive routine analysis of MP in food products is still not possible. In the present work, we present the development of a smart filter crucible as sampling and detection tool. After filtration and drying of the filtered-off solids, a direct determination of the MP mass content from the crucible sample can be done by thermal extraction desorption gas chromatography mass spectroscopy (TED-GC/MS). The new filter crucible allows a filtration of MP down to particle sizes of 5 µm. We determined MP contents below 0.01 µg/L up to 2 µg/L, depending on beverages bottle type. This may be directly related to the bottle type, especially the quality of the plastic material of the screw cap. Dependent on the plastic material, particle formation increases due to opening and closing operations during the use phase. However, we have also found that some individual determinations of samples were subjected to high errors due to random events. A conclusive quantitative evaluation of the products is therefore not possible at present. KW - Microplastic KW - TED-GC/MS KW - Plastic bottles KW - Bbeverages KW - Filter crucible PY - 2021 DO - https://doi.org/10.1080/19440049.2021.1889042 SN - 1944-0057 VL - 38 IS - 4 SP - 691 EP - 700 PB - Taylor & Francis AN - OPUS4-52323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Small-angle scattering for everyone: How to unlock the power of this ancient technique N2 - The obscure, yet fundamental technique of scattering can unlock essential information on the fine structure of materials. For you, it can help you understand how your batteries charge, how squid backbones work, or how hundreds of small variations in your syntheses affect your samples. As a nondestructive technique, it also measures your materials *in situ* or operando, as you pull it, heat it, electrify it, or align it one way or another. Scattering can be done using light, X-rays, neutrons, and even electrons, giving you the choice on which probe is best for you. The only downside? Scattering will always remain a complicated technique to do right. The technique gives you only one piece of information: the length distribution of density in your sample. How you interpret this (rather abstract) piece of information is up to you and your samples. Unlike microscopy, where the real-space image can be interpreted almost intuitively and artefacts are easier to spot, in scattering you cannot always easily identify artefacts. Therefore, the only way to do scattering experiments correctly is through rigour and care. For those of us with that particular eccentricity, seeing the rigour and care pay off is exhilarating, and opens the door to a life of happiness and excitement. This lecture will introduce scattering (in particular using X-rays and neutrons), what it is, what you can (and cannot) get out of it, and how to approach your scattering experiment. Regarding the experimental section, it will discuss the five parts that make up a successful scattering experiment based on real-life examples: Preparation: which and how you prepare your samples affects what you can get out of the interpretation Measurement: The machine design and your measurement choices dictates the final quality of your data Correction: Obtaining trustworthy scattering curves will greatly improve the speed and quality of your analysis. Analysis: Do you linearize, use generic scattering models, perform classical least-squares fitting, play with Monte-Carlo analysis or transform your data.. Some tips to help you make a choice. Interpretation: what does the analysis of all your samples tell you? Can you fit the puzzle pieces together to form a piece of knowledge? For further information, please feel free to explore the https://lookingatnothing.com/ weblog, the https://youtube.com/drheaddamage video channel, or by asking me in person or by email for specific questions at brian.pauw@bam.de . Some introductory reading can be found in the following papers: Pauw, B. R. (2013): Everything SAXS: small-angle scattering pattern collection and correction. _J. Phys.: Condens. Matter_ 25: 383201. DOI: [10.1088/0953-8984/25/38/383201](http://dx.doi.org/10.1088/0953-8984/25/38/383201) B. R. Pauw, A. J. Smith, T. Snow, N. J. Terrill, A. F. Thünemann, (2017): The modular SAXS data correction sequence for solids and dispersions, _Journal of Applied Crystallography_, 50: 1800–1811, DOI: [10.1107/S1600576717015096](https://doi.org/10.1107/S1600576717015096) G. J. Smales, B. R. Pauw (2021): The MOUSE project: a meticulous approach for obtaining traceable, wide-range X-ray scattering information. _Journal of instrumentation_ 16 (6) P06034. DOI: [10.1088/1748-0221/16/06/P06034](https://doi.org/10.1088/1748-0221/16/06/P06034) T2 - SAS School at the XIX International Small Angle Scattering Conference CY - Taipei, Taiwan DA - 02.11.2024 KW - X-ray scattering KW - Neutron scattering KW - Scattering KW - X-ray KW - Neutron KW - Introduction KW - Methodology PY - 2024 AN - OPUS4-61623 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 - INPR A1 - Ponader, Marco A1 - Röder, Bettina A1 - Paul, Martin A1 - Weller, Michael G. T1 - Sintered glass monoliths as new 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 minute. 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 nanofiltration step. The purity of the IgG was > 95% in one step and nearly 99% with a second polishing run. KW - Affinity Chromatography KW - Glass KW - Purification KW - Antibodies KW - Solid support KW - HPLC KW - FPLC KW - Separation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529117 DO - https://doi.org/10.20944/preprints202103.0298.v1 SN - 2310-287X N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M. SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-52911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmar, Stefan A1 - Weyrauch, Steffen A1 - Reemtsma, Thorsten A1 - Eisentraut, Paul A1 - Altmann, Korinna A1 - Ruhl, Aki S. A1 - Jekel, Martin T1 - Settling Velocities of Tire and Road Wear Particles: Analyzing Finely Graded Density Fractions of Samples from a Road Simulator and a Highway Tunnel N2 - The terminal settling velocity is considered the most critical parameter determining the transport of tire and road wear particles (TRWP) in aquatic environments. Nonetheless, no respective empirical data has been reported so far. In this study, particle samples from a road simulator and a highway tunnel were investigated with a validated imaging method. Different density and size fractions of both samples were measured separately, acquiring sizes and settling velocities of more than 30,000 individual particles. In addition, tire marker polymers were analyzed for each fraction via thermal extraction desorption-gas chromatography/mass spectrometry. Finally, the acquired particle data was combined according to the fractions’ estimated tire contents in order to deduce detailed probability distributions of particle size and settling velocity for the actual TRWP from both samples. Weighted by TRWP-incorporated tire mass, median diameters of 54 and 44 μm as well as median settling velocities of 0.65 and 0.22 mm/s were found for TRWP from the road simulator and highway tunnel, respectively. This study thus provides the first ever empirical data on TRWP settling velocities in water, which can be highly valuable input for modeling the environmental transport of TRWP and for dimensioning TRWP retention systems. KW - Microplastics KW - TED-GC/MS KW - Sinking velocities KW - Transport PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635449 DO - https://doi.org/10.1021/acs.est.5c04165 SN - 0013-936X VL - 59 IS - 26 SP - 13434 EP - 13446 PB - American Chemical Society (ACS) AN - OPUS4-63544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Separation of polystyrene nanoparticles bearing different carboxyl group densities and functional groups quantification with capillary electrophoresis and asymmetrical flow field flow fractionation N2 - Two sets of polystyrene nanoparticles (PSNPs) with comparable core sizes but different carboxyl group densities were made and separated using asymmetric flow field flow fractionation (AF4), capillary electrophoresis (CE), and the off-line hyphenation of both methods. Our results revealed the significant potential of two-dimensional off-line AF4-CE hyphenation to improve the separation and demonstrated for the first time, the applicability of CE to determine the functional group density of nanoparticles (NPs). Compared to the result acquired with conductometric titration, the result obtained with synthesized 100 nm sized PSNPs revealed only a slight deviation of 1.7%. Commercial 100 nm sized PSNPs yielded a deviation of 4.6 %. For 60 nm sized PSNPs, a larger deviation of 10.6 % between both methods was observed, which is attributed to the lower separation resolution. KW - Nanoparticle KW - A4F KW - Capillary electrophoresis KW - Carboxyl group PY - 2020 DO - https://doi.org/10.1016/j.chroma.2020.461392 VL - 1626 SP - 461392 PB - Elsevier B.V. AN - OPUS4-51080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Separation of polysterene nanoparticles with different coatings using 2D off-line coupling of asymmetrical flow field flow fractionation and capillary electrophoresis N2 - The successful off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) for Separation of nanoparticles (NPs) with different surface coatings was shown. Two mixtures of polystyrene nanoparticles (PS-NPs) with comparable core sizes (20 nm and 50 nm) but different coatings (no coating/carboxyl-coated) were studied. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional off-line coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots and can obviouly improve separation resolution. T2 - FFF 2020 CY - Wien, Austria DA - 23.02.2020 KW - Capillary electrophoresis KW - Nanoparticle PY - 2020 AN - OPUS4-50487 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 - RPRT A1 - Altmann, Korinna A1 - Abusafia, A A1 - Bannick, C-G A1 - Braun, U A1 - Crasselt, Claudia A1 - Dittmar, S A1 - Fuchs, M A1 - Gehde, M A1 - Hagendorf, C A1 - Heller, C A1 - Herper, D A1 - Heymann, S A1 - Kerndorff, A A1 - Knefel, M A1 - Jekel, M A1 - Lelonek, M A1 - Lunkenbein, T A1 - Obermaier, N A1 - Manhart, M A1 - Meurer, Maren A1 - Miclea, P-T A1 - Paul, A A1 - Richter, S A1 - Ricking, M A1 - Rohner, C A1 - Ruhl, A A1 - Sakai, Y A1 - Saravia Arzabe, C A1 - Scheid, C A1 - Schmitt, M A1 - Schnarr, M A1 - Schwertfirm, F A1 - Steinmetz, H A1 - Wander, Lukas A1 - Wiesner, Yosri A1 - Zechmeister, L T1 - RUSEKU - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt : Abschlussbericht N2 - 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. KW - Mikroplastik KW - Probennahme KW - TED-GC/MS KW - Fraktionierte Filtration KW - Mikroplastikreferenzmaterial PY - 2022 SP - 1 EP - 201 AN - OPUS4-57800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Falkenhagen, Jana A1 - Beskers, Timo. F. A1 - Myxa, Anett A1 - Pursch, Matthias T1 - Round-robin test for size exclusion chromatography – Data summary N2 - Size exclusion chromatography (SEC or GPC) is one critical component of polymer analysis to meet the increasing requirements in regulatory context – namely, determination of Mn, as well as oligomers of less than 500 g mol-1 and 1000 g mol-1. The underlying test methods (OECD 118/119 and DIN EN ISO 13885 1 to 3) provide a framework for SEC measurements; however, they lack sufficient specificity to obtain accurate results. Previous SEC round robin tests were mostly performed on homopolymers and did not collect data on oligomer contents. A new round robin test was initiated and conceptualized within the Task force “Method Evaluation for Polymer REACh (MeEP)”, an initiative of “Industrieforum Analytik” within the German Chemical Society (GDCh). Samples for this study were selected to represent both easy benchmark polymers as well as real-life, industry-relevant polymer materials. Data collection focused on the regulatory requirements. Distribution of samples, gathering of individual results and evaluation were carried out by BAM. A data summary as initial result is reported here. Further evaluation and interpretation are a part of ongoing research. KW - Size exclusion chromatography KW - Polymers KW - Oligomer content KW - Round-robin test PY - 2026 DO - https://doi.org/10.26272/opus4-65587 SP - 1 EP - 84 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-65587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kricheldorf, H. R. T1 - Reversible Polycondensations and the Jacobson-Stockmayer Theory N2 - Reversible polycondensations are polycondensations that include equilibration reactions at any stage of the process. Syntheses of Polyesters in bulk involving transesterification reactions and syntheses of polyamides in bulk involving transamidation are typical examples. In 1950, Jacobson and Stockmayer published a first theory of reversible polycondensations based on experimental studies with aliphatic polyesters.[1,2] They explained the reversibility by the reversible formation of cyclic oligomers and low molar mass polymers from an active chain end (so-called “back-biting”). The formation of cycles via end-to-end cyclization was excluded in agreement with Flory´s theory of irreversible polycondensations.[3] The reinvestigation of the Jacobson-Stockmayer experiments by the authors in combination with theoretical considerations shows that the JS theory is wrong. [4,5] It turned out that the experimental scenario is far from the reality. In real polycondensations, intermolecular equilibration is faster than “back-biting”, and end-to-end cyclization is quite normal. The revised theory of step-growth polymerization predicts that in the ideal case of 100% conversion, all reaction products are cycles, regardless, of whether the step-growth polymerization is reversible or not. T2 - Polycondensation 2024 CY - Lyon, France DA - 15.09.2024 KW - Polycondensation KW - Cyclisation KW - MALDI TOF MS PY - 2024 UR - https://polycond-2024.sciencesconf.org/ AN - OPUS4-61070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reifschneider, O. A1 - Vennemann, A. A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Hogeback, J A1 - Köppen, C. A1 - Großgarten, M. A1 - Sperling, M. A1 - Wiemann, M. A1 - Karst, U. T1 - Revealing Silver Nanoparticle Uptake by Macrophages Using SR-μXRF and LA-ICP-MS N2 - To better study the impact of nanoparticles on both in vitro and in vivo models, tissue distribution and cellular doses need to be described more closely. Here silver nanoparticles were visualized in alveolar macrophages by means of synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μXRF) with high spatial resolution of 3 × 3 μm2. For the spatial allocation of silver signals to cells and tissue structures, additional elemental labeling was carried out by staining with eosin, which binds to protein and can be detected as bromine signal with SR-μXRF. The method was compatible with immunostaining of macrophage antigens. We found that the silver distribution obtained with SR-μXRF was largely congruent with distribution maps from a subsequent laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of the same tissue sites. The study shows a predominant, though not exclusive uptake of silver into alveolar macrophages in the rat lung, which can be modeled by a similar uptake in cultured alveolar macrophages. Advantages and limitations of the different strategies for measuring nanoparticle uptake at the single cell level are discussed. KW - Synchrotron KW - BAMline KW - XRF KW - Nanoparticle KW - Macrophagen PY - 2020 DO - https://doi.org/10.1021/acs.chemrestox.9b00507 VL - 33 IS - 5 SP - 1250 EP - 1255 PB - American Chemical Society AN - OPUS4-50855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Results of the Plastic in the environment comparative test N2 - The talk describes the sturcture and the results of the "plastics in the environment" comparative test of 2019. T2 - Symposium "Challenges of microplastic analysis – Bridging state of the art and policy needs” CY - Online meeting DA - 09.09.2021 KW - Microplastic KW - Comparative test KW - ILC PY - 2021 AN - OPUS4-53236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt (RUSEKU) N2 - Der Vortrag wurde im Rahmen der Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF gehalten. Er fasst die Ergebnisse des Verbundprojektes RUSEKU zusammen. Es wurde die Herstellung verschiedener Testmaterialien für die Mikroplastik (MP) Analytik beschrieben. Im weiteren geht es um verschiedene Ansätze MP kostengünstig und schnell zu detektieren, z.B. mit Nahinfrarotspektroskopie. Nanoplastik konnte mit der Transmissionselektronenmikroskopie sichtbar gemacht werden. Für die praxisnahe Beprobung von Gewässern wurde die Fraktionierte Filtration entwickelt. Integrale Beprobungen können mit dem Sedimentationskasten erfolgen. Als Beispiele für die Beprobung realer Gewässer wurde das urbane Abwassersystem Kaiserslautern, Getränkewasser und Waschmaschinenwasser gezeigt. T2 - Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF CY - Online meeting DA - 20.04.2021 KW - Mikroplastik KW - TED-GC/MS KW - Probennahme KW - RUSEKU PY - 2021 AN - OPUS4-52546 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 - 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 - CONF A1 - Hahn, Marc Benjamin T1 - Reference Materials at BAM N2 - A introduction into reference materials, the certification process and brief over current reference projects at BAM is given. T2 - AK-Postdoc seminar CY - BAM Berlin, Germany DA - 02.02.2021 KW - Referenzmaterialien KW - Reference material KW - Homogeneity KW - Stability KW - Quality testing KW - Analytic KW - DNA KW - Dosimetry KW - Certification PY - 2021 AN - OPUS4-52060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Reference material candidates for microplastic analysis N2 - Every day, there are new headlines in the media about microplastics (1-1000 µm, ISO/TR 21960:2020) and nanoplastics (< 1 µm, ISO/TR 21960:2020) findings all over the planet with high variations in particle number and mass. The challenges in analytics are very complex, e.g. representative sampling, non-destructive sample preparation with concentrated particles and homogeneous distribution and true detection. All together lead to lacks in harmonization and results, which are hardly comparable. On the other hand, monitoring of microplastics is mandatory in the future strictly regulated by the EU commission in the Drinking water and Wastewater Framework Directive. One step to accurate and precise results will be the development of suitable reference materials mimicking particles in the environment. BAM developed test materials, which are produced by mixing a small portion of microplastic particles with a water-soluble matrix. After solid phase dilution and homogenisation small portions are pressed into tablets and bottled in glass vials (Figure 1). These tablets are well characterized with particle size distribution and SEM images. Additionally, they are tested as reference material candidate according to homogeneity and stability for particle number with µ-IR and µ-Raman as well as on particle mass with Py-GC/MS and TED-GC/MS after ISO Guide 35. Results are promising. The material passed the homogeneity control. No changes are observed within 6 months of storage. The same tested reference material is finally used in sample preparation experiments, where environmental suspended particular matter from surface water or baby milk powders are spiked with the tablets. T2 - ESOPS CY - Berlin, Germany DA - 09.09.2024 KW - Microplastics KW - TED-GC/MS KW - Reference materials KW - Polymer 3R KW - Tablets PY - 2024 AN - OPUS4-61017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Altmann, Korinna T1 - Reference material BAM-P206 polyethylene terephthalate (powder) N2 - 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. KW - Microplastic KW - Reference material KW - PET PY - 2023 DO - https://doi.org/10.26272/opus4-59778 SP - 1 EP - 23 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-59778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, UEA A1 - Streli, C. A1 - Radtke, Martin T1 - Reconstruction for coded aperture full-field x-ray fluorescence imaging N2 - 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. KW - Synchrotron KW - BAMline KW - Coded Aperture PY - 2022 SN - 1097-0002 VL - 65 SP - 57 EP - 70 PB - Cambridge University Press CY - Cambridge AN - OPUS4-56350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana T1 - Recent developments of X-ray absorption spectroscopy as analytical tool for biological and biomedical applications N2 - X-ray absorption spectroscopy (XAS), in its various modalities, has gained exponential attention and applicability in the field of biological and biomedical systems. Particularly in this field, challenges like low concentration of analyte or proneness to radiation damage have certainly settle the basis for further analytical developments, when using X-ray based methods. Low concentration calls for higher sensitivity—by increasing the detection limits (DL); while susceptibility for radiation damage requires shorter measurement times and/or cryogenic sample environment possibilities. This manuscript reviews the latest analytical possibilities that make XAS more and more adequate to investigate biological or biomedical systems in the last 5 years. KW - Biological & biomedical applications KW - TXRF-XAS KW - HERFD-XAS KW - RXES KW - Quick-XAS KW - Dispersive-XAS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531206 DO - https://doi.org/10.1002/xrs.3254 SN - 0049-8246 VL - 51 IS - 3 SP - 1 EP - 10 PB - John Wiley & Sons Ltd AN - OPUS4-53120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miclea, P.-T. T1 - Real-life airborne micro- and nano-plastic particles and fibres on a porous membrane filter system from a textile factory suitable for both: vibrational and mass spectrometry N2 - The poster presents an application of Si wafer filter system on indoor air sampling. A textile factory producing PP fibres was sampled. T2 - SETAC Europe 2023 CY - Dublin, Ireland DA - 30.04.2023 KW - Microplastics KW - Polymer 3R KW - Textile fibres KW - Si wafer filter KW - Microplastics sampling PY - 2023 AN - OPUS4-57462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Drago, Claudia T1 - Rapid sample preparation to detect microplastics in baby milk powder N2 - Microplastics, ubiquitous as it is, could be released into food during production chain, through packaging and by consumer´s use. To determinate human exposure to microplastics is crucial to monitor microplastics in food matrices. The current absence of standard sample preparation procedures to identify and quantify different microplastics according to number and mass have generate time-consuming protocols and lack of comparability among different analytical methods, laboratories and time scales. Monitoring microplastics in complex matrices as food, and in particular in baby milk powder, requires an accurate approach that need to be validate, to ensure the comparability of results. Bottled drinking water or surface waters, for example, can be measured with mass-based methods (TED-GC/MS or Py-GC/MS) directly after filtration. Baby milk powder, instead is more challenging, due to the proteins and fatty acid that clog the filters and contaminate the measuring devices with heavy carry over. In this study, we characterize the baby milk powder by thermogravimetric analysis (TGA) and we tested different treatments for matrix reduction: water, H2O2, citric acids. In particular, the use of citric acid was tested for protein reduction before filtration. Our hypothesis was that citric acid will induce the precipitation of proteins and amino acids, leading to a strong matrix reduction. In fact, this sample pre treatment, allowed us to use a higher intake, necessary for representative quantification. Finally, the milk powder was spiked with reference material tablets containing polyethylene terephthalate (PET). The PET was not degraded by the citric acid and high recovery rate was achieved by TED-GC/MS and Py-GC/MS methods. Considering the simplicity and accessibility of this sample preparation and its robust results, this procedure could be easily proposed as a simple sample preparation approach to monitor microplastics by mass-based methods. T2 - MICRO 2024 CY - Arrecife, Spain DA - 23.09.2024 KW - Microplastics KW - Milk KW - Polymer 3R KW - TED-GC/MS PY - 2024 AN - OPUS4-61273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falkenhagen, Jana A1 - Dalgic, Mete-Sungur A1 - Weidner, Steffen T1 - Quantitative MALDI-TOF Mass Spectrometry of Star-Shaped Polylactides Based on Chromatographic Hyphenation N2 - The end groups of three- and four-arm star-shaped polylactides (PLA) with trimethylolpropane and pentaerythritol core structures were functionalized with acetic acid. Reaction products with different degrees of functionalization were analyzed by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. Additional gradient elution liquid adsorption chromatography (GELAC) measurements were performed to determine the degree of functionalization. This technique enabled clear separation and sufficient quantification of the formed species. These chromatographic data could be used inversely to quantify mass spectrometric results, which are usually biased by the unknown ionization probabilities of different polymer end group structures. Our results showed that, in this particular case, the peak intensity in the MALDITOF mass spectra can be used to semiquantitatively determine the degree of functionalization in incompletely functionalized multiarm PLA. KW - Polylactides KW - MALDI-TOF-MS KW - Gradient elution liquid adsorption chromatography PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625292 DO - https://doi.org/10.1021/jasms.4c00491 SN - 1879-1123 SP - 1 EP - 9 PB - American Chemical Society (ACS) AN - OPUS4-62529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dalgic, Mete‐Sungur A1 - Kumar, Sourabh A1 - Weidner, Steffen T1 - Quantitative Analysis of Polymers by MALDI‐TOF Mass Spectrometry: Correlation Between Signal Intensity and Arm Number N2 - The signal intensities of linear and star‐shaped poly(L‐lactides) (PLA) and poly (ethylene oxides) (PEO) were compared to determine the influence of the number of arms on the ionization in matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF) mass spectrometry. In this study, a variety of blends were prepared and investigated, including binary and ternary combinations of linear and star‐shaped polymers with similar molecular masses. The focus was on examining their intensity ratios. In equimolar binary PLA blends, polymer stars were observed to exhibit higher intensities than their linear counterparts. This result was supported by experiments with equimolar ternary PLA blends, which clearly demonstrated an intensity dependence on the number of polymer arms. It was observed that four‐arm PLA exhibited higher intensities than three‐arm PLA. A similar trend was observed in investigations involving acetylated polymer end groups, suggesting that differences in ionization are primarily influenced by polymer architecture rather than end groups. In order to validate this assumption, the binding energies for [polymer‐K] + adduct ions utilizing the most stable geometry obtained from GOAT (Global Optimizer Algorithm) were calculated, revealing that star‐shaped lower mass oligomers have slightly higher binding energies. KW - MALDI-TOF MS KW - Starlike polymers KW - Quantification KW - Topology PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653401 DO - https://doi.org/10.1002/jms.70023 SN - 1076-5174 VL - 61 IS - 1 SP - 1 EP - 12 PB - John Wiley & Sons Ltd. AN - OPUS4-65340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Förste, F. A1 - Bauer, L. A1 - Streeck, C. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Kadow, D. A1 - Keil, C. A1 - Mantouvalou, I. T1 - Quantitative Analysis and 2D/3D Elemental Imaging of Cocoa Beans Using X‑ray Fluorescence Techniques N2 - 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. KW - BAMline KW - Synchrotron KW - XRF KW - CXC KW - Cocoa PY - 2023 DO - https://doi.org/10.1021/acs.analchem.2c05370 VL - 95 SP - 5627 EP - 5635 PB - ACS Publications AN - OPUS4-57832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Quantifying the total and accessible amount of surface functionalities and ligands on nano-materials: Overview and recommended methods N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage. NP function, interaction with biological species, and environmental fate are largely determined by surface functionalities. This calls for reliable, reproducible, and standardized surface characterization methods, which are vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Validated and standardized workflows for surface analysis are also increasingly requested by industry, international standardization organizations, regulatory agencies, and policymakers. To establish comparable measurements of surface functionalities across different labs and ease instrument performance validation, reference test materials and reference materials of known surface chemistry as well as reference data are needed. In the following, different methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques are presented and discussed regarding method-inherent advantages and limitations. Special emphasis is dedicated to traceable quantitative nuclear magnetic resonance (qNMR), X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. T2 - LNE Workshop CY - Paris, France DA - 04.11.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Characterization KW - Advanced material KW - Surface KW - Standardization KW - Reference material KW - Functional group KW - Quantification KW - Coating KW - Automation KW - Potentiometry KW - Method KW - Validation KW - Optical assay KW - Fluram KW - Fluorescamine KW - qNMR KW - Comparison KW - ILC PY - 2025 AN - OPUS4-64726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tavernaro, Isabella A1 - Rajotte, Isabelle A1 - Thibeault, Marie-Pier A1 - Sander, Philipp C. A1 - Kodra, Oltion A1 - Lopinski, Gregory A1 - Radnik, Jörg A1 - Johnston, Linda J. A1 - Brinkmann, Andreas A1 - Resch-Genger, Ute T1 - Quantifying surface groups on aminated silica nanoparticles of different size, surface chemistry, and porosity with solution NMR, XPS, optical assays, and potentiometric titration N2 - We assessed the quantification of surface amino functional groups (FGs) for a large set of commercial and custom-made aminated silica nanoparticles (SiO2 NPs) with sizes of 20–100 nm, prepared with different sol–gel routes, different amounts of surface amino FGs, and different porosity with four methods providing different, yet connected measurands in a bilateral study of two laboratories, BAM and NRC, with the overall aim to develop standardizable measurements for surface FG quantification. Special emphasis was dedicated to traceable quantitative magnetic resonance spectroscopy (qNMR) performed with dissolved SiO2 NPs. For the cost efficient and automatable screening of the amount of surface amino FGs done in a first step of this study, the optical fluorescamine assay and a potentiometric titration method were utilized by one partner, i.e., BAM, yielding the amount of primary amino FGs accessible for the reaction with a dye precursor and the total amount of (de)protonatable FGs. These measurements, which give estimates of the minimum and maximum number of surface amino FGs, laid the basis for quantifying the amount of amino silane molecules with chemo-selective qNMR with stepwise fine-tuned workflows, involving centrifugation, drying, weighting, dissolution, measurement, and data evaluation steps jointly performed by BAM and NRC. Data comparability and relative standard deviations (RSDs) obtained by both labs were used as quality measures for method optimization and as prerequisites to identify method-inherent limitations to be later considered for standardized measurement protocols. Additionally, the nitrogen (N) to silicon (Si) ratio in the near-surface region of the SiO2 NPs was determined by both labs using X-ray photoelectron spectroscopy (XPS), a well established surface sensitive analytical method increasingly utilized for microparticles and nano-objects which is currently also in the focus of international standardization activities. Overall, our results underline the importance of multi-method characterization studies for quantifying FGs on NMs involving at least two expert laboratories for effectively identifying sources of uncertainty, validating analytical methods, and deriving NM structure–property relationships. KW - Advanced Materials KW - Amino Groups KW - Calibration KW - Characterization KW - Functional groups KW - Method Comparison KW - Nano Particle KW - Validation KW - XPS KW - Optical Assay KW - Quantification KW - Surface Analysis KW - Reference Materials KW - Synthesis KW - Fluorescence PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649992 DO - https://doi.org/10.1039/d5na00794a VL - 7 IS - 21 SP - 6888 EP - 6900 PB - Royal Society of Chemistry AN - OPUS4-64999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Qualitätssicherung bei der Analyse von Mikroplastik per TED GC/MS N2 - Die Thermo Extraktion Desorption Gas Chromatograpie Massen Spektrometrie (TED-GC/MS) ist ein schnelles thermoanalytisches Verfahren zur Bestimmung von Gehalten an Mikroplastik (MP). Die Kombination aus teils schwerflüchtigen Analyten und Kältebrücken führt zu Memory-Effekten, denen u.a. durch häufige Blindwertmessungen begegnet werden muss. Reduzierte Probedurchsätze sind die Folge. Um Messergebnisse abzusichern und den Gerätestatus bei gleichzeitig hoher Messleistung überwachen zu können, wurde die sequentielle Standardmethode überarbeitet. T2 - Tagung der Wasserchemischen Gesellschaft 2022 CY - Online meeting DA - 23.05.2022 KW - Mikroplastik KW - Thermoanalytik KW - TED-GC/MS KW - Qualitätssicherung PY - 2022 AN - OPUS4-55087 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Portesi, C. T1 - qNMR for standardised measurements of surface functionalities on nanoparticles N2 - Engineered nanoparticles have a large application potential in fields such as medicine, sensing, catalysis, energy storage, and opto-electronics [1]. The applicability and performance of engineered nanoparticles is largely determined by their surface chemistry, i.e. functional groups and ligands on the particle surface. However, documented standards to quantify functional groups and ligands currently do not exist. Such standards are required to support quality control of nanomaterial production and surface modification processes, and safe-by-design concepts and to meet regulatory requirements. Here, this issue is addressed by developing and standardizing quantitative Nuclear Magnetic Resonance (qNMR) methods for the characterization of surface functionalized nanoparticles which specifically address the determination of the amount and chemical composition of surface functionalities and coatings. This work is being developed under the EMP project 23NRM02 SMURFnano - Standardised measurements of surface functionalities on nanoparticles. qNMR competence of 7 qNMR laboratories involved in the project was first tested with a molecular model sample i.e. citrate, to be assessed in terms of purity. Citrate is often used as hydrophilic surface ligand for different nanoparticles. Then, the first nanoparticle samples, here a set of aminated SiO2 NPs [1] with a particle size of 100 nm and two amino group densities, prepared and characterized by BAM regarding size and surface charge as well as stability over 21 months with an optical assay and qNMR, were assessed in an international interlaboratory comparison (ILC) on qNMR. Thereby, the amount of surface amino groups introduced by grafting of the silica cores with different amounts of 3-aminopropyl)triethoxysilane (APTES) was quantified by each participant following a sample preparation protocol previously developed by BAM and NRC.The results of the ILC were then used to refine the protocol for sample preparation and to identify critical points for qNMR measurement and data analysis. This work will contribute to the development of a Preliminary Work Item (PWI) 19257 (ISO/TC 229) on surface functional groups and coatings on nano-objects. Also, it will lay the groundwork to perform ILCs on the quantification and determination of the amount of surface functional groups under the roof of VAMAS TWA2 (Surface Chemical Analysis) for different types of nanomaterials possessing industry-relevant surface functionalities using qNMR. These ILCs will be complemented by other techniques like X-Ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). T2 - BERM CY - Halifax, Canada DA - 01.06.2025 KW - Quality assurance KW - Nano KW - Particle KW - Synthesis KW - Advanced materials KW - Characterization KW - Electron microscopy KW - Silica KW - Surface KW - qNMR KW - Optical assay KW - Interlaboratory comparison KW - Metrology KW - Validation KW - Standardization PY - 2025 AN - OPUS4-63443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Booth, A. T1 - Production of a 1-10 μm polypropylene reference material for development of analytical methods N2 - The poster is about the preparation of microplastics in the size range of 1-10 µm. These size range of particles can be inhalded and therefore be toxic for humans. The preparation is done by comminution of PP pellets and sieving. Characterisation occured for size with laser diffraction, for type with FTIR and for shape with SEM. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Reference materials PY - 2025 AN - OPUS4-63367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Processing and application properties of multiple principal element alloys (MPEA) N2 - 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. T2 - FAU-Department Werkstoffwissenschaften, Seminar: Aktuelle Probleme der Werkstoffwissenschaften CY - Erlangen, Germany DA - 25.04.2024 KW - Welding KW - Application properties KW - Machining KW - High-entropy alloy KW - Hydrogen PY - 2024 AN - OPUS4-59975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Preliminary results of an interlaboratory comparison on microplastics organised by plasticsfate N2 - 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. T2 - CUSP annual meeting and conference CY - Utrecht, Netherlands DA - 12.09.2023 KW - Microplastics KW - TED-GC/MS KW - Polymer 3R KW - Reference material KW - ILC on detection methods PY - 2023 AN - OPUS4-60036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Richter, Silke A1 - Hoppe, Marion A1 - Meckelburg, Angela A1 - Prinz, Carsten A1 - Roik, Janina A1 - Abad Andrade, Carlos Enrique T1 - Powering precision: development of a certified reference material for elemental composition analysis of lithium nickel manganese cobalt oxide (Li-NMC) cathode material for lithium-ion batteries N2 - This work presents the development and certification of the world’s first certified reference material (CRM), BAM-S014, for a lithium nickel manganese cobalt oxide (LiNi0.33Mn0.33Co0.33O2 or Li-NMC 111) cathode material—an integral component in high-energy-density lithium-ion batteries that power electric vehicles (EVs), portable electronics, and stationary energy storage systems. By providing certified mass fractions for 11 elements, this CRM addresses a critical need for accurate and traceable elemental analysis, supporting quality control and regulatory compliance in the global battery industry. Ensuring reliable and harmonized measurements supports the efficient use of resources, including the reuse of recycled materials, and ultimately helps maintain product performance and safety. The values were assigned through an interlaboratory comparison involving 16 participating laboratories and various analytical techniques such as inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence (XRF) spectrometry, and combustion analysis. In addition to chemical characterization, the certification process includes homogeneity and stability testing of the candidate material. Details are provided on the analytical methods used for chemical characterization and the calculation of the uncertainties of the certified mass fractions. In addition to detailing the development of the CRMs, this work provides an overview of ongoing standardization activities in Li-component analysis, thereby guiding the calibration of analytical methods and contributing to the establishment of globally accepted standards for evaluating energy storage materials and advancing sustainable mobility and clean energy solutions. KW - Certified reference material KW - Lithium nickel manganese cobalt oxide KW - LNMC KW - Lithium-ion battery KW - Cathode material PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643763 DO - https://doi.org/10.1007/s00216-025-05766-7 SN - 1618-2642 VL - 417 IS - 12 SP - 2643 EP - 2653 PB - Springer Nature AN - OPUS4-64376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen T1 - Polymerization of L‐Lactide Catalyzed by Metal Acetylacetonate Complexes N2 - ABSTRACTRing‐opening polymerizations (ROPs) of l‐lactide (LA) were performed at 120°C, 140°C, 150°C, and 180°C in bulk catalyzed by acetylacetonate (acac) complexes of manganese(II), nickel(II), copper(II), zirconium(IV), dibutyltin(IV), and vanadyl(V). These experiments revealed that only the acac complexes of Zr and Bu2Sn were reactive enough to enable quantitative polymerization within a few hours. Further ROPs with Bu2Sn(acac)2 and Zr(acac)4 showed that Bu2Sn(acac)2 had a slightly lower reactivity than the Zr complex. The ROPs catalyzed with Zr(acac)4 yielded number average molecular weights (Mn) up to 70,000 g mol−1. The matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF) mass spectra indicated an exclusive formation of cycles in the mass range of up to m/z 13,000 for Zr(acac)4 and up to m/z 18,000 for Bu2Sn(acac)2. Unusually high melting temperatures (187°C–192°C) were also achieved along with high crystallinities. Furthermore, four lactide/glycolide copolymerizations catalyzed by Zr(acac)4 were performed, and the topology and the extent of transesterification were characterized by MALDI‐TOF mass spectrometry and 13C NMR spectroscopy. KW - MALDI-TOF MS KW - Polycondensation KW - Acetylacetonate PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639754 DO - https://doi.org/10.1002/pol.20250788 SN - 2642-4150 SP - 1 EP - 9 PB - Wiley Periodicals LLC. AN - OPUS4-63975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Meyer, A. A1 - Falkenhagen, Jana A1 - Kricheldorf, H. R. T1 - Polycondensations and Cyclization of Poly(L-lactide) Ethyl Esters in the Solid State N2 - 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. KW - Polylactide KW - MALDI-TOF MS KW - Crystalinity PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-592934 DO - https://doi.org/10.1039/d3py01232h SN - 1759-9962 VL - 15 IS - 2 SP - 71 EP - 82 PB - RSC Publ. CY - Cambridge AN - OPUS4-59293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Scheliga, Felix A1 - Kricheldorf, Hans R. T1 - Polycondensation, Cyclization and Disproportionation of Solid Poly(L-lactide) Trifluoroethyl Esters and the Simultaneous Formation of Extended Chain Crystals and Extended Ring Crystals N2 - Two poly(L-lactide)s (PLAs) with a degree of polymerization (DP) of 20 or 100 were prepared by trifluoroethanol-initiated ring-opening polymerization (ROP) catalyzed by tin(II) 2-ethyl hexanoate (SnOct2). These PLAs were annealed at 140 ◦C or at 160 ◦C in the presence of SnOct2, and the changes in topology and molecular weight distribution (MWD) were monitored by matrix-assisted laser desorption/ionization time-of flight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC). For the PLA with a DP 20, the main reaction was polycondensation combined with higher dispersities. In the case of the DP 100, PLA polycondensation was combined with disproportionation and the formation of a new MWD maximum around m/z 3500. In addition, extensive cyclization occurred, and the resulting cyclic PLAs crystallized separately from the linear chains in the form of extended ring crystals. These results also suggest that both extended chain and extended ring crystals posses the same crystal thickness as a result of thermodynamically controlled transesterification in the solid state. KW - Polycondensation KW - MALDI KW - Polylactide KW - Cyclization PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616441 DO - https://doi.org/10.1016/j.polymer.2024.127800 VL - 315 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-61644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen A1 - Scheliga, Felix T1 - Polycondensation of L-lactic acid: a deeper look into solid state polycondensation N2 - L-Lactic acid (LA) was condensed in the presence of SnCl2 or 4-toluenesulfonic acid (TSA) at 140 °C, and chain growth without cyclization was observed. In addition, poly(L-lactic acid)s (PLAs) with a degree of polymerization (DP) of 25, 50 or 100 were prepared by water-initiated ring-opening polymerization (ROP). These PLAs were annealed in the solid state at 140 °C and 160 °C in the presence of tin(II) 2-ethylhexanoate (SnOct2, SnCl2 or TSA). The changes in the molar mass distribution and in the topology were characterized by means of matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry and size exclusion chromatography (SEC). With increasing time, fewer side reactions caused higher molar masses and increasing fractions of cyclic polylactides (cPLA) were obtained. Their “saw tooth” pattern in the MALDI-TOF mass spectra indicated the formation of extended ring crystallites in the solid state. TSA was the most active catalyst and caused fewer side reactions than SnCl2, which was the least reactive catalyst. Acetylation of the CH-OH end groups hindered polycondensation and prevented the formation of cPLAs. Reaction mechanisms will be discussed. KW - MALDI-TOF MS KW - Polycondensation KW - Polylaktide KW - Solid state PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625271 DO - https://doi.org/10.1039/d4py01191k SN - 1759-9962 SP - 1 EP - 9 PB - Royal Society of Chemistry (RSC) AN - OPUS4-62527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Plastik in Böden: Mikroplastik-Ergebnisse N2 - In diesem Vortrag geht um die Vorstellung der Ergebnisse des UBA Projektes Plastik in Böden. Es werden Mikroplastik-Gehalte in verschiedenen Böden präsentiert. T2 - Fachgespräch "Plastik in Böden" CY - Online meeting DA - 28.03.2022 KW - Mikroplastik KW - Mikroplastik Böden KW - Mikroplastik-Analytik PY - 2022 AN - OPUS4-54648 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Plastik in Böden: Mikroplastik-Analytik N2 - Im Vortrag wir eine Methode zur Analyse von Mikroplastik in Böden dargestellt. Es geht dabei um die Probenvorbereitung und Detektion. T2 - Fachgespräch "Plastik in Böden" CY - Online meeting DA - 28.03.2022 KW - Mikroplastik KW - TED-GC/MS KW - Mikroplastik-Analytik KW - Methodenentwicklung Böden PY - 2022 AN - OPUS4-54646 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - PlasticTrace WP1 – Stakeholder Workshop N2 - The talk summarizes the achievments of WP1 of the PlasticTrace project. Microplastic reference materials were developed by producing tablets. Different preparation methods were compared. Characterisation of the tablets was done after filtration with µFTIR, QCL, µRaman, Py-GC/MS and TED-GC/MS after ISO standards ISO 16094-2 and ISO/FDIS 16094-3. Polymer types are polypropylene and polyethylene terephthalate. T2 - Stakeholder Workshop PlasticsTrace CY - Online meeting DA - 09.09.2025 KW - Microplastics KW - Reference materials KW - TED-GC/MS KW - PET PY - 2025 AN - OPUS4-64258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - PE-Rezyklat Einsatz in Gefahrgutbehältern? N2 - In diesem Vortrag geht es darum zu beschreiben, ob Rezyklat für PE Behälter gefüllt mit Gefahrgut Anwendung finden darf. Kanister aus Neuware und Rezyklat wurden verschiedenen Untersuchungen unterzogen. Es wurde der Feststoff und Leachable getestet. Methoden sind TED-GC/MS und GC-HRMS. Proben der Leachable wurden nach 1 und 4 Wochen genommen und die Peakanzahl vergleichen dargestellt. Als Lösemittel wurden Wasser, Ethanol, EtOAc, Ammoniak und HNO3 verwendet. T2 - Fachaustausch Projekt GeSKAR CY - Dessau, Germany DA - 10.01.2025 KW - Gefahrgutbehälter KW - Rezyklat PY - 2025 AN - OPUS4-62396 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Putzu, Mara A1 - Wiesner, Yosri A1 - Weimann, Christiane A1 - Hodoroaba, Vasile-Dan A1 - Muniategui Lorenzo, Soledad A1 - Fernández-Gonzáles, Verónica A1 - Booth, Andy M. A1 - Igartua, Amaia A1 - Benismail, Nizar A1 - Coïc, Laureen A1 - Chivas-Joly, Carine A1 - Fenoglio, Ivana A1 - Rossi, Andrea Mario A1 - Giovannozzi, Andrea Mario A1 - Altmann, Korinna T1 - Optimization of tablet processing as a reference material for microplastic detection methods N2 - Reference materials (RMs) are essential and highly demanded tools for the development and validation of methods for microplastic (MP) quantification in complex matrices, to ensure comparable and harmonized approaches aligned with EU commission criteria for monitoring MPs (e.g., Drinking Water Directive and Urban Wastewater Treatment Directive). This study investigates different approaches for optimizing the production of polypropylene (PP) RMs in the form of water-soluble tablets, which were carefully evaluated for their homogeneity and stability according to ISO Guide 30, ISO 33401, and ISO 33405. PP particles (1–100 μm) were produced by cryomilling and embedded in a lactose/PEG matrix, then pressed into tablets (18 µg theoretical PP mass). The production process was optimized by varying (i) the size distribution of the matrix components and (ii) the mixer instrument. The materials obtained were characterized by thermogravimetric analysis to assess the homogeneity distribution of MPs with respect to PP mass in the individual tablets and their stability over a 4-month period. The most promising approach, with a homogenous mass of 19 μg (standard deviation of 4 μg), relative standard deviation of 19%, was further investigated for homogeneity by comparison with thermo-analytical mass determination methods, such as TED-GC/MS (thermal extraction desorption-gas chromatography/mass spectrometry) and Py-GC/MS (pyrolysis-gas chromatography-mass spectrometry), and for number-based characterization using micro-Raman spectroscopy. Material characterization was also examined using laser diffraction, scanning electron microscopy, and ATR-FTIR. Based on the results, the optimized processing protocol yields a PP RM suitable for quality control and method performance studies supporting standardization. KW - Microplastics KW - TED-GC/MS KW - Reference materials KW - Polypropylene PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653290 DO - https://doi.org/10.1007/s00216-025-06271-7 SN - 1618-2642 SP - 1 EP - 14 PB - Springer Science and Business Media LLC AN - OPUS4-65329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Putzu, Mara T1 - Optimization of production process for microplastics reference materials N2 - Microplastics (MP) are defined as plastic particles mainly consisting of polymers in the size range of 1 to 1000 µm. They can be found in a wide range of environmental matrices but also in food products, indicating a potential risk on humans and environment. Plastic debris in the environment or food chain are extremely complex in terms of size, concentration, polymer type, levels of physiochemical degradation and undefined morphologies which makes their isolation and detection in complex matrices challenging. Analytical detection methods and techniques to identify and quantify microplastics in environmental and food matrices are numerous but validated and standardized methods are currently lacking. To close this research gap, reference materials (RMs) and representative sample preparation approaches are urgently needed. Homogeneity and stability are two crucial characteristics for the certification process of the reference materials. For this purpose, we aim to present ways to prepare reference materials containing very low masses of close-to reality plastic particles with broad size distribution (10-100 µm) that are homogeneously distributed in tablet-to-tablet variation and stable over time. Our work is based on the ISO Guide 30:2015 and ISO Guide 35:2017 to fulfil the criteria set in future standards ISO/DIS 16094-2 and ISO/DIS 16094-3. The property of interest will be the mass detected by thermogravimetric analysis (TGA). Furthermore, informative values will be achieved by mass-based technique TED-GC/MS and spectroscopic microscopy techniques, such as µ-FTIR spectroscopy and µ-Raman. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Reference materials KW - TED-GC/MS PY - 2025 AN - OPUS4-63386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Cakir, Cafer Tufan T1 - Optimization of depth resolved X-ray absorption spectroscopy in grazing emission mode for characterizing compositionally complex alloys N2 - Layered materials are fundamental to technological advancements, offering distinct properties that differentiate them from bulk materials. In electronics, for instance, thin-film transistors (TFTs) are used to enhance charge transport and flexibility, thereby improving device performance. In the same way, thin-film photovoltaic devices used in renewable energy use strategic layering to absorb light more efficiently and separate electron-hole pairs more effectively, which leads to higher energy conversion efficiency. In recent decades, the development of new alloys has highlighted the importance of layered materials in another context. Compositionally complex alloys, for example, form multiple oxide layers on their surfaces when they oxidize. Studying these corrosion layers is crucial for understanding material-environment interactions. Typical surface analysis techniques, including X-ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS), and Meitner-Auger electron spectroscopy (MAES), provide valuable insights but are constrained by their requirements for high Vacuum conditions and their limited depth analysis. In contrast, X-ray absorption near-edge structure (XANES) spectroscopy presents a versatile and advantageous alternative. It operates effectively under ambient conditions and allows time-resolved measurements, enhancing the analysis of materials in real-time as they undergo structural and compositional changes. This adaptability broadens the scope for material analysis, allowing for a more comprehensive understanding of dynamic processes. Grazing Emission X-ray Fluorescence (GEXRF) spectroscopy stands out as a nondestructive, depth-resolved, element-specific characterization technique important for collecting depth-resolved information at the nanometer scale. Its ability to collect in-Depth resolved information based on the grazing emission angle of the fluorescence Radiation makes it ideal for investigating thin films, corrosion layers, and interfaces within layered materials. The integration of XANES in emission mode with GEXRF enables detailed exploration of the chemical states of the analyzed atom and provides depth-resolved information. This study discusses grazing emission X-ray absorption near-edge structure spectroscopy (GEXANES), a novel layer analysis technique that is created by integrating these two methods. This study also innovatively combines machine learning with GEXANES spectroscopy to reduce experimental times. By using active learning, a subset of machine learning, it refines the data acquisition process, enabling more efficient and streamlined methods. The application of active learning in this context illustrates the potential of data-driven approaches to transform experimental methodologies, particularly in resource-limited environments such as synchrotron facilities, thereby accelerating scientific research and discovery. KW - Angle resolved XRF KW - GEXRF KW - BO KW - Active Learning KW - XRF PY - 2025 DO - https://doi.org/10.34726/hss.2025.101302 SP - 1 EP - 129 CY - Technische Univeristät Wien AN - OPUS4-63793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Eisentraut, Paul A1 - Altmann, Korinna T1 - One Year Observation of Microplastic Concentrations in the River Rhine N2 - In recent years, the quantification of microplastics (MP) in aquatic environments has gained increasing attention, particularly regarding their environmental distribution and potential exposure levels. Environmentally relevant exposure data are still essential for a realistic risk assessment of the harmful health potential of microplastics in freshwater systems. This study addresses a large data set of MP concentrations analyzed and processed under statistical aspects and provides mass concentrations as well as associated size fractions of the detected MP. Over a 12 month period, samples were collected at three locations and analyzed across three particle size fractions (100−500 μm, 50−100 μm, and 10−50 μm) using thermalextraction desorption-gas chromatography/mass spectrometry (TED-GC/MS). The most prevalent polymers identified were polyethylene (PE), polypropylene (PP), polystyrene (PS), styrene−butadiene rubber (SBR), and natural rubber (NR). Statistical analyses, including principal component and cluster analysis, revealed size-dependent patterns,minor seasonal variation and spatial variations. These findings are particularly significant for ecotoxicological research and regulatory development, especially regarding tire abrasion a rarely quantified but potentially harmful MP source. The study contributes aluable data for future environmental monitoring and supports EU directives on wastewater and drinking water quality KW - TED-GC/MS KW - Microplastics KW - Environment KW - Monitoring KW - Reference data PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654669 DO - https://doi.org/10.1021/acsestwater.5c00530 SN - 2690-0637 SP - 1 EP - 10 PB - American Chemical Society (ACS) AN - OPUS4-65466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miclea, P.-T. T1 - Novel laser pre-structured silicon filters for microplastics analysis N2 - This research presents a novel laser-assisted approach to silicon filter fabrication, offering an effective alternative to traditional photolithographic processes. By integrating selective femtosecond laser irradiation with photoelectrochemical etching, we achieved precisely controlled pore geometries, overcoming common challenges in filter production for microplastic and nanoscale filtration suitable for microplastic number and mass analysis. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Nanoplastics KW - Raman microspectroscopy PY - 2025 AN - OPUS4-63384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - News from the BAMline N2 - A presentation of recent measurements at the BAMline with focus on AI and ML applications T2 - Seminar: Strahlenphysikalische Anwendungen in Technik und Medizin CY - Vienna, Austria DA - 18.05.2022 KW - Synchrotron KW - BAMline KW - Bayesian Statistics KW - Gold KW - X-ray fluorescence PY - 2022 AN - OPUS4-56253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trimpin, Sarah A1 - Yenchick, Frank S. A1 - Lee, Chuping A1 - Hoang, Khoa A1 - Pophristic, Milan A1 - Karki, Santosh A1 - Marshall, Darrell D. A1 - Lu, I-Chung A1 - Lutomski, Corinne A. A1 - El-Baba, Tarick J. A1 - Wang, Beixi A1 - Pagnotti, Vincent S. A1 - Meher, Anil K. A1 - Chakrabarty, Shubhashis A1 - Imperial, Lorelei F. A1 - Madarshahian, Sara A1 - Richards, Alicia L. A1 - Lietz, Christopher B. A1 - Moreno-Pedraza, Abigail A1 - Leach, Samantha M. A1 - Gibson, Stephen C. A1 - Elia, Efstathios A. A1 - Thawoos, Shameemah M. A1 - Woodall, Daniel W. A1 - Jarois, Dean R. A1 - Davis, Eric T.J. A1 - Liao, Guochao A1 - Muthunayake, Nisansala S. A1 - Redding, McKenna J. A1 - Reynolds, Christian A. A1 - Anthony, Thilani M. A1 - Vithanarachchi, Sashiprabha M. A1 - DeMent, Paul A1 - Adewale, Adeleye O. A1 - Yan, Lu A1 - Wager-Miller, James A1 - Ahn, Young-Hoon A1 - Sanderson, Thomas H. A1 - Przyklenk, Karin A1 - Greenberg, Miriam L. A1 - Suits, Arthur G. A1 - Allen, Matthew J. A1 - Narayan, Srinivas B. A1 - Caruso, Joseph A. A1 - Stemmer, Paul M. A1 - Nguyen, Hien M. A1 - Weidner, Steffen A1 - Rackers, Kevin J. A1 - Djuric, Ana A1 - Shulaev, Vladimir A1 - Hendrickson, Tamara L. A1 - Chow, Christine S. A1 - Pflum, Mary Kay H. A1 - Grayson, Scott M. A1 - Lobodin, Vladislav V. A1 - Guo, Zhongwu A1 - Ni, Chi-Kung A1 - Walker, J. Michael A1 - Mackie, Ken A1 - Inutan, Ellen D. A1 - McEwen, Charles N. T1 - New Processes for Ionizing Nonvolatile Compounds in Mass Spectrometry: The Road of Discovery to Current State-of-the-Art N2 - This Perspective covers discovery and mechanistic aspects aswell as initial applications of novel ionization processes for use in massspectrometry that guided us in a series of subsequent discoveries, instrumentdevelopments, and commercialization. Vacuum matrix-assisted ionization onan intermediate pressure matrix-assisted laser desorption/ionization sourcewithout the use of a laser, high voltages, or any other added energy wassimply unbelievable, at first. Individually and as a whole, the variousdiscoveries and inventions started to paint, inter alia, an exciting new pictureand outlook in mass spectrometry from which key developments grew thatwere at the time unimaginable, and continue to surprise us in its simplisticpreeminence. We, and others, have demonstrated exceptional analyticalutility. Our current research is focused on how best to understand, improve, and use these novel ionization processes throughdedicated platforms and source developments. These ionization processes convert volatile and nonvolatile compounds from solid orliquid matrixes into gas-phase ions for analysis by mass spectrometry using, e.g., mass-selected fragmentation and ion mobilityspectrometry to provide accurate, and sometimes improved, mass and drift time resolution. The combination of research anddiscoveries demonstrated multiple advantages of the new ionization processes and established the basis of the successes that lead tothe Biemann Medal and this Perspective. How the new ionization processes relate to traditional ionization is also presented, as wellas how these technologies can be utilized in tandem through instrument modification and implementation to increase coverage ofcomplex materials through complementary strengths. KW - Mass spectrometry PY - 2024 DO - https://doi.org/10.1021/jasms.3c00122 SN - 1879-1123 VL - 35 IS - 12 SP - 2753 EP - 2784 PB - American Chemical Society (ACS) AN - OPUS4-61417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Nanocarriers – Challenges Imposed by Material Characterization N2 - A brief perspective of BAM on nanocarriers is presented including examples with special emphasis on the characterization of such materials and underlying challenges. In this respect, also ongoing activities at BAM on different types of core/shell nanomaterials and related systems are briefly summarized. T2 - Kolloquium BfR CY - Online meeting DA - 18.03.2021 KW - Nanomaterial KW - Nanocarrier KW - Size KW - Surface chemistry KW - Release kinetics KW - Chemical composition KW - Core/shell nanoparticle KW - Quantum dot KW - Spectroscopy KW - Fluorescence PY - 2021 AN - OPUS4-52412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Drexel, R. T1 - Nano-sized Polypropylene as a Promising Candidate Reference Material: Preparation, Characterization and Stability in Complex Matrices N2 - The lack of nanoplastic (NPs) reference materials capable of mimicking real-world scenarios is currently hampering the development of validated extraction techniques from complex matrices (e.g. soils, sediments, biota), the development of analytical approaches for robust identification and quantification, and the ability to use environmentally relevant test materials in (eco)toxicity testing and hazard assessment [1]. The large body of available data suggests that larger microplastics (MPs) in the natural environment are irregular shaped, partially degraded (chemically and physically), a continuum of sizes, shapes and densities, represent a wide range of polymer types, and acts as a reservoir for thousands of plastic chemicals. Although NPs have been described as being neither MPs nor engineered nanoparticles [2], and while direct measurement data of true NP in the environment remain elusive, they are expected to be as equally diverse as MPs [3]. Here, we present a strategy towards the development of a potential NP reference material based on nano-sized polyproplyene particles (nanoPP) developed within the EURAMET-funded PlasticTrace project (https://plastictrace.eu/). The strategy includes the preparation, the physicochemical characterization and the stability assessment of nanoPP in suspension both in its pristine state, but also when spiked into food (mineral water and milk) and environmental matrices (suspended particulate matter collected from the river Elbe ). Collected experimental data suggests nanoPP to be a promising candidate for a NP reference material. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Nanoplastics KW - Reference materials PY - 2025 AN - OPUS4-63382 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 - CONF A1 - Altmann, Korinna A1 - Braun, U. T1 - Monitoring von Mikroplastik N2 - Der Vortrag gibt einen Überblick was bei der Analyse von Mikroplastik zu beachten ist und beschreibt die Vor- und Nachteile der TED-GC/MS. T2 - Abschlusstreffen MikroPlaTas CY - Online meeting DA - 23.06.2021 KW - Mikroplastik KW - TED-GC/MS KW - Mikroplastik-Analytik PY - 2021 AN - OPUS4-52916 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - ML@BAMLINE N2 - An overview of the machine learning methods used at BAMline. Examples of automatic alignment and optimisation based on Gaussian processes are discussed. Quantification of XRF measurements and reconstruction for coded aperture imaging based on neural networks are also presented. T2 - Machine Learning Workshop BAM CY - Online meeting DA - 18.03.2021 KW - Artificial Intelligence KW - Machine learning KW - Bayesian Optimization KW - Gaussian process KW - Neural Network PY - 2021 AN - OPUS4-54142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Mikroplastikanalytik mittels TED-GC/MS: H/D-Austausch an Zersetzungsprodukten von D-markiertem Polystyrol als interner Standard N2 - Deuteriertes Polystyrol (D-PS) verbessert die Mikroplastikdetektion mit der TED-GC/MS, u.a. durch höhere Reproduzierbarkeit. Es ist kostengünstig (0,1 ct/Analyse) und durch die gute Löslichkeit (z.B. in Toluol) schnell und reproduzierbar zu dosieren. Bestimmte Matrices führen jedoch zu einem Austausch des Deuteriums durchWasserstoff. Das Poster zeigt das Messprinzip, bei welchen Matrices H/D-Austausch erfolgt, Ergebnisse von Kinetikuntersuchungen sowie Möglichkeiten, den Austausch zu verhindern oder zu umgehen. T2 - Tagung der Wasserchemischen Gesellschaft CY - Online Meeting DA - 10.05.2021 KW - Mikroplastik KW - Analyse KW - Interner Standard KW - H/D-Austausch PY - 2021 AN - OPUS4-52727 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik – Ein Problem für die Menschheit? N2 - Mikroplastik findet sich in Ozeanen, Seen, Flüssen und Bächen. Es kann in unserem Boden, in der Luft und sogar in Organismen nachgewiesen werden. Jedes Jahr werden weltweit Millionen Tonnen freigesetzt. Doch wo und wie landet Mikroplastik in der Umwelt? Und wie können wir diese winzigen Partikel nachweisen? T2 - Berlin Science Week CY - Berlin, Germany DA - 01.11.2021 KW - Mikroplastik KW - TED-GC/MS PY - 2021 AN - OPUS4-53734 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik heute: Was haben wir in den letzten Jahren erreicht? N2 - In diesem Vortrag geht es um eine Übersicht über die Thematik der Mikroplastik, Was ist Mikroplastik, wie entsteht es und wo kommt es her. Es wird beschrieben wie eine repräsentative Probenahme erfolgen kann und wie welche Herausforderungen bei der Probenvorbereitung existieren. Die Detektion wird ausführlich beschrieben, sowohl mit Partikelanzahl als auch Masse. Im weiteren werden erste Referenzmaterialien und ihre Anwendung in internationalen Ringversuchen beschrieben. Der zweite Teil zeigt die Normungsaktivitäten im Bereich der Mikroplastik. T2 - Mitgliederversammlung der GdCh Lackchemie CY - Online Meeting DA - 20.09.2024 KW - Mikroplastik KW - TED-GC/MS KW - Polymer 3R KW - Reference material KW - ILC on detection methods PY - 2024 AN - OPUS4-61087 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik Detektion mit Thermoanalytischen Methoden: Analytik, Referenzmaterial, Ringversuche N2 - 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. T2 - Plastik, Mikroplastik, Nanopartikel, PFAS und Verunreinigungen (Agilent Workshop) CY - Hamburg, Germany DA - 28.05.2024 KW - Mikroplastik KW - TED-GC/MS KW - Polymer 3R KW - Ringversuche KW - Referenzmaterial PY - 2024 AN - OPUS4-60155 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik an der BAM: TED-GC/MS und Referenzmaterialien N2 - Thema ist die Funktionsweise der TED-GC/MS als Methode für die Mikroplastik-Detektion sowie die Herstellung dazugehöriger Referenzmaterialien an der BAM T2 - 25. Kolloquium Massenspektrometrie von Polymeren CY - Online meeting DA - 17.06.2021 KW - Mikroplastik KW - TED-GC/MS KW - Referenzmaterial PY - 2021 AN - OPUS4-52835 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Kerndorff, A. A1 - Ricking, M. A1 - Bednarz, M. A1 - Obermaier, N. A1 - Lukas, M. A1 - Asenova, M. A1 - Bordós, G. A1 - Eisentraut, Paul A1 - Hohenblum, P. A1 - Hudcova, H. A1 - Humer, F. A1 - István, T. G. A1 - Kirchner, M. A1 - Marushevska, O. A1 - Nemejcová, D. A1 - Oswald, P. A1 - Paunovic, M. A1 - Sengl, M. A1 - Slobodnik, J. A1 - Spanowsky, K. A1 - Tudorache, M. A1 - Wagensonner, H. A1 - Liska, I. A1 - Braun, U. A1 - Bannick, C. G. T1 - Microplastics in the Danube River Basin: A First Comprehensive Screening with a Harmonized Analytical Approach N2 - In this study, carried out within the Joint Danube Survey 4, a comprehensive microplastic screening in the water column within a large European river basin from its source to estuary, including major tributaries, was realized. The objective was to develop principles of a systematic and practicable microplastic monitoring strategy using sedimentation boxes for collection of suspended particulate matter followed by its subsequent analysis using thermal extraction desorption-gas chromatography/mass spectrometry. In total, 18 sampling sites in the Danube River Basin were investigated. The obtained suspended particulate matter samples were subdivided into the fractions of >100 μm and <100 μm and subsequently analyzed for microplastic mass contents. The results showed that microplastics were detected in all samples, with polyethylene being the predominant polymer with maximum contents of 22.24 μg/mg, 3.23 μg/mg for polystyrene, 1.03 μg/mg for styrene-butadiene-rubber, and 0.45 μg/mg for polypropylene. Further, polymers such as different sorts of polyester, polyacrylates, polylactide, and natural rubber were not detected or below the detection limit. Additional investigations on possible interference of polyethylene signals by algae-derived fatty acids were assessed. In the context of targeted monitoring, repeated measurements provide more certainty in the interpretation of the results for the individual sites. Nevertheless, it can be stated that the chosen approach using an integrative sampling and determination of total plastic content proved to be successful. KW - Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), monitoring KW - Microplastics KW - River KW - Suspended particulate matter (SPM) KW - Sedimentation box (SB) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551444 DO - https://doi.org/10.1021/acsestwater.1c00439 VL - 2 IS - 7 SP - 1174 EP - 1181 PB - ACS Publications AN - OPUS4-55144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Microplastics at BAM: TED-GC/MS and reference materials N2 - Thsi talk aims to present the activities of microplastic analysis at BAM according to TED-GC/MS and reference materials developement. T2 - Webinar BAM / University of Birmingham CY - Online meeting DA - 15.06.2021 KW - Microplastic KW - TED-GC/MS KW - Reference materials PY - 2021 AN - OPUS4-53738 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bauer, J. A1 - Miclea, P.-T. A1 - Braun, U. A1 - Altmann, Korinna A1 - Turek, M. A1 - Hagendorf, C. T1 - Microplastic detection and analysis in water samples N2 - 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. T2 - International Conference on Sustainable Energy-Water-Environment Nexus in Desert Climate 2019 CY - Ar-Rayyan, Qatar DA - 02.12.2019 KW - Microplastics KW - Water samples PY - 2022 SP - 111 EP - 113 PB - Springer AN - OPUS4-56240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Microplastic analysis using TED-GC/MS: H/D-Exchange of decomposition products of D-marked polystyrene as an internal standard N2 - Deuterated polystyrene (D-PS) improves microplastic detection with TED-GC / MS, among other things through higher reproducibility. It is inexpensive (0.1 ct / analysis) and can be dosed quickly and reproducibly thanks to its good solubility (e.g. in toluene). However, certain matrices lead to an exchange of the deuterium with hydrogen. The poster shows the measuring principle, in which matrices H/D-exchange takes place, the results of kinetic studies and ways of preventing or circumventing the H/D-exchange. T2 - SALSA MAKE AND MEASURE 2021 CY - Online meeting DA - 16.09.2021 KW - Microplastic KW - H/D-Exchange KW - Internal Standard KW - TED-GC/MS KW - Thermoanalytic PY - 2021 AN - OPUS4-53681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miclea, Paul T1 - Microanalysis of Airborne Nano/Microplastic Particles in an Textile Industrial Environment N2 - Micro- and nanoplastics (MNPs) are emerging global contaminants, present in air, soil, and water. The textile industry is potentially a major contributor, releasing synthetic particles like polyamide, polyester, and acrylic during production. This study assessed MNP levels outside and inside a textile-processing facility using online air samplers with silicon (Si) and quartz filters. Real-time particle counts (PM0.3–PM10) were obtained via a laser detector. Si filters (9 mm, 10/1 µm pores) and quartz filters (25 mm, 1.2 µm pores, pre-calcined at 800°C) were used for sampling. Custom holders allowed selective sampling for PM10 and PM1 on Si filters. Sampling conditions included a 3-hour collection at 2 L/min (GilAir Plus pump) starting at 7:00 AM (T1) and 2:00 PM (T2), with intermittent ventilation, 23.3 °C average temperature, and 52.5% humidity. Particle weights collected (µg) were: quartz – 4.9E-05 (T1), 5.1E-05 (T2); Si – 3.2E-05 (T1), 5E-06 (T2). Outside particle counts ranged from 3,584 (T1) to 15,165 (T2); inside: 9,901 (T1) to 12,921 (T2). Maximum indoor PM10 and PM0.3 levels were 72/m³ and 71,979/m³, respectively. Particles were analyzed using electron microscopy and µRaman spectroscopy, confirming high concentrations of irregularly shaped PP-based particles (1–5 µm). T2 - 12th TEXTEH CY - Bucharest, Romania DA - 23.10.2025 KW - Microplastics KW - Airborne particles KW - Raman microspectroscopy PY - 2025 AN - OPUS4-64485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miclea, P.-T. T1 - Micro- and nanoplastic particle number and mass-based analysis on a plastic-free size-selective two stage Si membrane filtration cascade N2 - The poster presents a Si wafer filter development as two stage cascade and the adapter for microplastics filtration. T2 - SETAC Europe 2023 CY - Dublin, Ireland DA - 30.04.2023 KW - Microplastics KW - Filtration KW - TED-GC/MS KW - Polymer 3R KW - Cascade filtration PY - 2023 AN - OPUS4-57461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Visileanu, Emilia A1 - Catalin Grosu, Marian A1 - Tiberiu Miclea, Paul A1 - Altmann, Korinna A1 - Brossell, Dirk T1 - Methods for the collection and characterization of airborne particles in the textile industry N2 - Airborne particulate matter is one of the main air pollutants. Their impact on mortality, and the occurrence of pulmonary and cardiovascular complications, have been the subject of numerous studies. Airborne particles are complex mixtures of organic and inorganic substances from different sources of particle emissions. Particulate Matter (PM) particles are classified according to their aerodynamic diameter expressed in µm and can vary from coarse (PM 10) to fine (less than PM 2.5). These diameter considerations are fundamental because they condition the penetration of particles into the bronchopulmonary system and the body. In recent years, there has been an interest in so-called “ultra-fine” particles, with a diameter of 0.1 µm (or 100 nm), or PM 0.1. They are nanoparticles and their impact on human health is not yet clear.With more than 1.5 million employees, textiles and clothing is a diverse sector that plays an important role in the European manufacturing industry, producing a turnover of €162 billion.An important component of the solid particles that generate air pollution in the textile industry is microplastics (MP) and nano plastics (NP), which also include microfibers (<5mm) and nanofibers (<100 nm), respectively. The particles released into the air during fiber and yarn processing range from 1 µg/m3 to 50 µg/m3.The paper presents the results of the determination of indoor and outdoor air concentration levels in textile companies, to identify the areas with the highest concentration level, by using an online recording system such as the Laser Aerosol Spectrometer MINI LAS model 11-E. The total concentration level TSP (µg/m3), the fractions PM 10(µg/m3), PM 2.5(µg/m3), PM1(µg/m3), as well as the total number of particles TC (1/l), were shown. It was noted that TSP is approximately at the same level both indoors and outdoors, but the fractions of PM10, PM2.5, and PM1 have much higher values indoors than outdoors with possible consequences on workers' health.The next step was the collection of fibers, namely micro and nano plastic particles from the vicinity of the workplaces of polyester, polyamide, and polypropylene fibers processing units in the textile industry in Romania, to obtain a sufficient quantity for laboratory analysis to determine the size and shape of the particles as well as their chemical composition. Two types of pumps were used, differentiated by their operating parameters: TECORA SKYPOST with airflow of 38 l/min and GILAIRPLUS with airflow 2l/min. Filters made of different materials with different diameters and pore sizes were used, namely: quartz filters (ø 47 mm, and ø 37 mm) on a TECORA SKYPOST type pump, polycarbonate nucleopore coated with a gold membrane (ø 25 mm) and silica filter (ø 9 mm) on GILAIRPLUS type pump.Using descriptive statistics, the calculation of correlation coefficients highlighted a strong correlation between the variables: "Collected mass/ Air concentration" and "Collected mass/ Air volume" for all diameters of the filters.The highest collected particle volume, determined by weighing the filters before and after collection, was obtained with the quartz filters (ø 47 mm) at an airflow of 38 l/min. The particles collected (polyester, polyamide, polypropylene) in the first stage were analyzed by SEM and thermogravimetric and it was found that the quartz filters absorbed the particles inside, with very few remaining on the surface. Thus no known methods can be used to perform analysis for particles collected on quartz filters. The number of particles on the filters was insufficient for analysis either because of the collection parameters used or because of the loss of particles during transport. As a result, in the next step, the use of 9 mm Si filters using the GILAIRPLUS pump at an airflow rate of 2l/min was chosen.To improve the transport conditions and avoid the loss of the particles and keep them on the surface of the filters, two methods were applied:- after weighing the filters were reintroduced into the collection pump holder;- a filtration system for airborne micro-nano plastics was designed and manufactured to selectively collect and transport PM10 and PM1 particles collected on SI filters.In both cases, SEM, Raman mapping, and GS-MS microscopy were used for analysis.Several times more PM10 than PM1 (74.5µg compared to 12.5 µg) was found. In all cases, both particles and fibers showed the same Raman fingerprint.The GS-MS analyses showed some contamination of the workspaces with particles other than the processed fibers. The presence of non-notifiable substances was also observed.The most viable filters are Si filters with a pore size of 10 microns to 1 micron and the use of the selected collection and transport filter system. In the following a filter system will be applied for collection on Au membrane-coated polycarbonate filters. T2 - 5th International Conference on Human Systems Engineering and Design: Future Trends and Applications (IHSED 2023) KW - Microplastics KW - Textiles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624442 DO - https://doi.org/10.54941/ahfe1004132 VL - 112 SP - 212 EP - 223 PB - AHFE International AN - OPUS4-62444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - 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 - CONF A1 - Weidner, Steffen T1 - MALDI Mass spectrometry of synthetic polymers – making molecular elephants to fly N2 - The importance of MALDI TOF mass spectrometry for the analysis of synthetic polymers is shown and some specific issues influencing the analysis e.g. polymer mass dispersity, matrix and matrix homogeneity, nature of cations and end groups, sequence distribution are discussed by means of examples. T2 - Merck Polymer Seminar CY - Online meeting DA - 29.04.2021 KW - MALDI-ToF MS KW - Ionization KW - Desorption KW - Polymers PY - 2021 AN - OPUS4-52545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Yue A1 - Colnaghi, Timoteo A1 - Gong, Yilun A1 - Zhang, Huaide A1 - Yu, Yuan A1 - Wei, Ye A1 - Gan, Bin A1 - Song, Min A1 - Marek, Andreas A1 - Rampp, Markus A1 - Zhang, Siyuan A1 - Pei, Zongrui A1 - Wuttig, Matthias A1 - Ghosh, Sheuly A1 - Körmann, Fritz A1 - Neugebauer, Jörg A1 - Wang, Zhangwei A1 - Gault, Baptiste T1 - Machine learning‐enabled tomographic imaging of chemical short‐range atomic ordering N2 - In solids, chemical short‐range order (CSRO) refers to the self‐organization of atoms of certain species occupying specific crystal sites. CSRO is increasingly being envisaged as a lever to tailor the mechanical and functional properties of materials. Yet quantitative relationships between properties and the morphology, number density, and atomic configurations of CSRO domains remain elusive. Herein, it is showcased how machine learning‐enhanced atom probe tomography (APT) can mine the near‐atomically resolved APT data and jointly exploit the technique's high elemental sensitivity to provide a 3D quantitative analysis of CSRO in a CoCrNi medium‐entropy alloy. Multiple CSRO configurations are revealed, with their formation supported by state‐of‐the‐art Monte‐Carlo simulations. Quantitative analysis of these CSROs allows establishing relationships between processing parameters and physical properties. The unambiguous characterization of CSRO will help refine strategies for designing advanced materials by manipulating atomic‐scale architectures. KW - Chemical short-range order (CSRO) KW - Atom probe tomography (APT) KW - Machine learning PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623777 DO - https://doi.org/10.1002/adma.202407564 SN - 1521-4095 VL - 36 IS - 44 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-62377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning: examples from BAMline N2 - Various applications for artificial intelligence in the context of spectroscopy will be presented. in particular, examples from BAMline will be presented. After a short introduction to synchrotron radiation, artificial intelligence algorithms for the quantification of X-ray fluorescence measurement are discussed. In the second example, information retrieval by natural language processing is discussed. T2 - Analytical Academy CY - Online meeting DA - 02.06.2020 KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron PY - 2020 AN - OPUS4-51898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning for direct quantification of XRF measurements N2 - In this talk I’ll describe the use of artificial neural networks (ANN) for quantifying X-ray fluorescence (XRF) measurements. The main idea of this talk is to give an overview of the process needed to generate a model that can then be applied to a specific problem. In XRF, a sample is excited with X-rays and the resulting characteristic radiation is detected to determine elements quantitatively and qualitatively. This is traditionally done in several time-consuming steps. I’ll show the possibilities and problems of using a neural network to realise a "one-click" quantification. This includes generating training data using Monte Carlo simulation and augmenting the existing data set with an ANN to generate more data. The search for the optimal hyperparameters, manually and automatically, is also described. For the case presented, we were able to train a network with a mean absolute error of 0.1% by weight for the synthetic data and 0.7% by weight for a set of experimental data obtained with certified reference materials. T2 - Seminar series: Artificial Intelligence applied to X-ray / synchrotron techniques CY - Online meeting DA - 24.06.2021 KW - Artificial intelligence KW - Machine learning KW - Synchrotron KW - XRF PY - 2021 AN - OPUS4-54140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Rakotondrajoa, A. T1 - Machine learning based quantification of synchrotron radiation-induced X-ray fluorescence measurements - a case study N2 - In this work, we describe the use of artificial neural networks for the quantification of X-ray fluorescence measurements. The training data were generated using Monte Carlo simulation, which avoided the use of adapted reference materials. The extension of the available data set by means of an ANN to generate additional data was demonstrated. Particular emphasis was put on the comparability of simulated and experimental data and how the influence of deviations can be reduced. The search for the optimal hyperparameter, manual and automatic, is also described. For the presented case, we were able to train a network with a mean absolute error of 0.1 weight percent for the synthetic data and 0.7 weight percent for a set of experimental data obtained with certified reference materials. KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron KW - Neural network PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519008 DO - https://doi.org/10.1088/2632-2153/abc9fb SP - 1 EP - 16 PB - IOP Publishing AN - OPUS4-51900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning - Examples from BAM Line N2 - This talk explores applications of artificial intelligence in the field of spectroscopy, with a special focus on research conducted at BAMline. We begin with an overview of synchrotron radiation and its unique capabilities in material analysis. The first part of the talk will cover the integration of AI algorithms in quantifying X-ray fluorescence measurements, providing enhanced precision and efficiency in data analysis. Following this, we will examine the role of language models in spectroscopic research, showcasing how these tools can facilitate the control of complex experimental set-ups T2 - Analytical Academy CY - Berlin, Germany DA - 12.11.2024 KW - ChatGPT KW - Neural networks KW - XRF KW - Synchrotron KW - BAMline PY - 2024 AN - OPUS4-61698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Lösemittelfreie Probenpräparation zur Untersuchung von Polymerblends mittels MALDI-TOF MS N2 - 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. T2 - 28. Kolloquium - Massenspektrometrische Techniken zur Untersuchung synthetischer Polymere CY - Berlin, Germany DA - 14.05.2024 KW - Polymere KW - Massenspektrometrie KW - Probenpräparation PY - 2024 AN - OPUS4-60032 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Weidner, Steffen T1 - Low Molar Mass Cyclic Poly(L-lactide)s: Separate Transesterification Reactions of Cycles and Linear Chains in the Solid State N2 - L-Lactide (LA) was polymerized with neat tin(II) 2-ethylhexanoate (SnOct2) in toluene at 115 °C at low concentration with variation of the LA/Cat ratio. Cyclic polylactides (cPLAs) with number average molecular weights (Mn) between 7 000 and 17 000 were obtained. MALDI-TOF mass spectrometry also revealed the formation of a few percent of linear chains. Crystalline cPLAs with Mn around 9 000 and 14 000 were annealed at 140 °C in the presence of ScOct2 or dibutyl-2-stanna-1,3-dithiolane (DSTL). Simultaneously, crystallites of extended linear chains and crystallites of extended cycles were formed regardless of the catalyst, indicating that transesterification reaction proceeded different for linear chains and for cycles, governed by thermodynamic control. The formation of extended chain crystallites with low dispersity indicates the existence of symproportionation of short and long chains. A complementary experiment was carried out with a PLA ethyl ester composed mainly of linear chains with a small fraction of cycles KW - Polylactide KW - MALDI-TOF MS KW - Annealing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606228 DO - https://doi.org/10.1039/D4SM00567H SN - 1744-6848 SP - 1 EP - 12 PB - Royal Society of Chemistry (RSC) AN - OPUS4-60622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -