TY - JOUR
A1 - Koch, Matthias
A1 - Mauch, Tatjana
A1 - Riedel, Juliane
T1 - Development of a Hydrazine-Based Solid-Phase Extraction and Clean-Up Method for Highly Selective Quantification of Zearalenone in Edible Vegetable Oils by HPLC-FLD
N2 - Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the Fusarium mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47–494 μg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part).
KW - Mycotoxin
KW - Food
KW - Reversible covalent hydrazine chemistry (RCHC)
KW - Quantitative determination
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554812
DO - https://doi.org/10.3390/toxins14080549
VL - 14
IS - 8
PB - MDPI
CY - Basel
AN - OPUS4-55481
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Epping, Ruben
A1 - Lisec, Jan
A1 - Koch, Matthias
T1 - Changes in Black Truffle (Tuber melanosporum) Aroma during Storage under Different Conditions
N2 - The enticing aroma of truffles is a key factor for their culinary value. Although all truffle species tend to be pricy, the most intensely aromatic species are the most sought after. Research into the aroma of truffles encompasses various disciplines including chemistry, biology, and sensory science. This study focusses on the chemical composition of the aroma of black truffles (Tuber melanosporum) and the changes occurring under different storage conditions. For this, truffle samples were stored under different treatments, at different temperatures, and measured over a total storage time of 12 days. Measurements of the truffle aroma profiles were taken with SPME/GC–MS at regular intervals. To handle the ample data collected, a systematic approach utilizing multivariate data analysis techniques was taken. This approach led to a vast amount of data which we made publicly available for future exploration. Results reveal the complexity of aroma changes, with 695 compounds identified, highlighting the need for a comprehensive understanding. Principal component analyses offer initial insights into truffle composition, while individual compounds may serve as markers for age (formic acid, 1-methylpropyl ester), freshness (2-Methyl-1-propanal; 1-(methylthio)-propane), freezing (tetrahydrofuran), salt treatment (1-chloropentane), or heat exposure (4-hydroxy-3-methyl-2-butanone). This research suggests that heat treatment or salt contact significantly affects truffle aroma, while freezing and cutting have less pronounced effects in comparison. The enrichment of compounds showing significant changes during storage was investigated with a metabolomic pathway analysis. The involvement of some of the enriched compounds on the pyruvate/glycolysis and sulfur pathways was shown.
KW - Mass Spectrometry
KW - Metabolomics
KW - Tuber melanosporum
KW - Truffle Aroma
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601731
DO - https://doi.org/10.3390/jof10050354
VL - 10
IS - 5
SP - 1
EP - 22
PB - MDPI
AN - OPUS4-60173
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Reiber, T.
A1 - Hübner, Oskar
A1 - Dose, C.
A1 - Yushchenko, D. A.
A1 - Resch-Genger, Ute
T1 - Fluorophore multimerization on a PEG backbone as a concept for signal amplification and lifetime modulation
N2 - Fluorescent labels have strongly contributed to many advancements in bioanalysis, molecular biology, molecular imaging, and medical diagnostics. Despite a large toolbox of molecular and nanoscale fluorophores to choose from, there is still a need for brighter labels, e.g., for flow cytometry and fluorescence microscopy, that are preferably of molecular nature. This requires versatile concepts for fluorophore multimerization, which involves the shielding of dyes from other chromophores and possible quenchers in their neighborhood. In addition, to increase the number of readout parameters for fluorescence microscopy and eventually also flow cytometry, control and tuning of the labels’ fluorescence lifetimes is desired. Searching for bright multi-chromophoric or multimeric labels, we developed PEGylated dyes bearing functional groups for their bioconjugation and explored their spectroscopic properties and photostability in comparison to those of the respective monomeric dyes for two exemplarily chosen fluorophores excitable at 488 nm. Subsequently, these dyes were conjugated with anti-CD4 and anti-CD8 immunoglobulins to obtain fluorescent conjugates suitable for the labeling of cells and beads. Finally, the suitability of these novel labels for fluorescence lifetime imaging and target discrimination based upon lifetime measurements was assessed. Based upon the results of our spectroscopic studies including measurements of fluorescence quantum yields (QY) and fluorescence decay kinetics we could demonstrate the absence of significant dye-dye interactions and self-quenching in these multimeric labels. Moreover, in a first fluorescence lifetime imaging (FLIM) study, we could show the future potential of this multimerization concept for lifetime discrimination and multiplexing.
KW - Imaging
KW - Quantum yield
KW - Quality assurance
KW - Antibody
KW - Conjugate
KW - Cell
KW - FLIM
KW - PEG
KW - Flow cytometry
KW - Lifetime
KW - Energy transfer
KW - Quantitative spectroscopy
KW - Nano
KW - Particle
KW - Fluorescence
KW - Dye
KW - Amplification
KW - Microscopy
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602197
DO - https://doi.org/10.1038/s41598-024-62548-4
SN - 2045-2322
VL - 14
IS - 1
SP - 1
EP - 11
AN - OPUS4-60219
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wegner, Karl David
A1 - Resch-Genger, Ute
T1 - The 2023 Nobel Prize in Chemistry: Quantum dots
N2 - The 2023 Nobel Prize in Chemistry was awarded to Aleksey I. Ekimov (prize share 1/3), Louis E. Brus (prize share 1/3), and Moungi G. Bawendi (prize share 1/3) for groundbreaking inventions in the field of nanotechnology, i.e., for the discovery and synthesis of semiconductor nanocrystals, also termed quantum dots, that exhibit size-dependent physicochemical properties enabled by quantum size effects. This feature article summarizes the main milestones of the discoveries and developments of quantum dots that paved the road to their versatile applications in solid-state lighting, display technology, energy conversion, medical diagnostics, bioimaging, and image-guided surgery.
KW - Quantum dots
KW - Semiconductor nanocrystals
KW - Luminescence
KW - Quantitative spectroscopy
KW - Quantum yield
KW - Advanced nanomaterials
KW - Quality assurance
KW - Energy transfer
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597843
DO - https://doi.org/10.1007/s00216-024-05225-9
VL - 2024
SP - 1
EP - 11
PB - Springer
CY - Cham
AN - OPUS4-59784
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fiedler, Saskia
A1 - Frenzel, Florian
A1 - Würth, Christian
A1 - Tavernaro, Isabella
A1 - Grüne, M.
A1 - Schweizer, S.
A1 - Engel, A.
A1 - Resch-Genger, Ute
T1 - Interlaboratory Comparison on Absolute Photoluminescence Quantum Yield Measurements of Solid Light Converting Phosphors with Three Commercial Integrating Sphere Setups
N2 - Scattering luminescent materials dispersed in liquid and solid matrices and luminescent powders are increasingly relevant for fundamental research and industry. Examples are luminescent nano- and microparticles and phosphors of different compositions in various matrices or incorporated into ceramics with applications in energy conversion, solid-state lighting, medical diagnostics, and security barcoding. The key parameter to characterize the performance of these materials is the photoluminescence/fluorescence quantum yield (Φf), i.e., the number of emitted photons per number of absorbed photons. To identify and quantify the sources of uncertainty of absolute measurements of Φf of scattering samples, the first interlaboratory comparison (ILC) of three laboratories from academia and industry was performed by following identical measurement protocols. Thereby, two types ofcommercial stand-alone integrating sphere setups with different illumination and detection geometries were utilized for measuring the Φf of transparent and scattering dye solutions and solid phosphors, namely, YAG:Ce optoceramics of varying surface roughness, used as converter materials for blue light emitting diodes. Special emphasis was dedicated to the influence of the measurement geometry, the optical properties of the blank utilized to determine the number of photons of the incident excitation light absorbed by the sample, and the sample-specific surface roughness. While the Φf values of the liquid samples matched between instruments, Φf measurements of the optoceramics with different blanks revealed substantial differences. The ILC results underline the importance of the measurement geometry, sample position, and blank for reliable Φf data of scattering the YAG:Ce optoceramics, with the blank’s optical properties accounting for uncertainties exceeding 20%.
KW - Nano
KW - Fluorescence
KW - Reference material
KW - Luminescence
KW - Quantitative spectroscopy
KW - Particle
KW - Quantum yield
KW - Quality assurance
KW - Phosphor
KW - Converter material
KW - Lifetime
KW - Interlaboratory comparison
KW - Method
KW - Uncertainty
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600945
DO - https://doi.org/10.1021/acs.analchem.4c00372
SN - 0003-2700
SP - 6730
EP - 6737
PB - ACS Publications
AN - OPUS4-60094
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - López-Iglesias, C.
A1 - Markovina, A.
A1 - Nirmalananthan-Budau, N.
A1 - Resch-Genger, Ute
A1 - Klinger, D.
T1 - Optically monitoring the microenvironment of a hydrophobic cargo in amphiphilic nanogels: influence of network composition on loading and release
N2 - Amphiphilic nanogels (ANGs) are promising carriers for hydrophobic cargos such as drugs, dyes, and catalysts.
Loading content and release kinetics of these compounds are controlled by type and number of hydrophobic groups in the amphiphilic copolymer network. Thus, understanding the interactions between cargo and colloidal carrier is mandatory for a tailor-made and cargo-specific ANG design. To systematically explore the influence of the network composition on these interactions, we prepared a set of ANGs of different amphiphilicity and loaded these ANGs with varying concentrations of the solvatochromic dye Nile Red (NR). Here, NR acts as a hydrophobic model cargo to optically probe the polarity of its microenvironment. Analysis of the NR emission spectra as well as measurements of the fluorescence quantum yields and decay kinetics revealed a decrease in the polarity of the NR microenvironment with increasing hydrophobicity of the hydrophobic groups in the ANG network and dye–dye interactions at higher loading concentrations. At low NR concentrations, the hydrophobic cargo NR is encapsulated in the hydrophobic domains. Increasing NR concentrations resulted in probe molecules located in a more hydrophilic environment, i.e., at the nanodomain border, and favored dye–dye interactions and NR aggregation.
These results correlate well with release experiments, indicating first NR release from more hydrophilic network locations. Overall, our findings demonstrate the importance to understand carrier–drug interactions for efficient loading and controlled release profiles in amphiphilic nanogels.
KW - Particle
KW - Energy transfer
KW - Limit of detection
KW - Polymer
KW - Luminescence
KW - Quantitative spectroscopy
KW - Nano
KW - Quantum yield
KW - Lifetime
KW - Quality assurance
KW - Dye
KW - Probe
KW - Sensor
KW - Nile Red
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601603
DO - https://doi.org/10.1039/d4nr00051j
SN - 2040-3364
IS - 16
SP - 9525
EP - 9535
PB - The Royal Society of Chemistry
AN - OPUS4-60160
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tavernaro, Isabella
A1 - Matiushkina, Anna
A1 - Rother, Kai Simon
A1 - Mating, Celina
A1 - Resch-Genger, Ute
T1 - Exploring the potential of simple automation concepts for quantifying functional groups on nanomaterials with optical assays
N2 - Until now, automation in nanomaterial research has been largely focused on the automated synthesis of engineered nanoparticles (NPs) including the screening of synthesis parameters and the automation of characterization methods such as electron microscopy. Despite the rapidly increasing number of NP samples analyzed due to increasing requirements on NP quality control, increasing safety concerns, and regulatory requirements, automation has not yet been introduced into workflows of analytical methods utilized for screening, monitoring, and quantifying functional groups (FGs) on NPs. To address this gap, we studied the potential of simple automation tools for the quantification of amino surface groups on different types of aminated NPs, varying in size, chemical composition, and optical properties, with the exemplarily chosen sensitive optical fluorescamine (Fluram) assay. This broadly applied, but reportedly error-prone assay, which utilizes a chromogenic reporter, involves multiple pipetting and dilution steps and photometric or fluorometric detection. In this study, we compared the influence of automated and manual pipetting on the results of this assay, which was automatically read out with a microplate reader. Special emphasis was dedicated to parameters like accuracy, consistency, achievable uncertainties, and speed of analysis and to possible interferences from the NPs. Our results highlight the advantages of automated surface FG quantification and the huge potential of automation for nanotechnology. In the future, this will facilitate process and quality control of NP fabrication, surface modification, and stability monitoring and help to produce large data sets for nanomaterial grouping approaches for sustainable and safe-by-design, performance, and risk assessment studies.
KW - Automation
KW - Quantification of amino groups
KW - Fluorescamine assay
KW - Amorphous silica nanoparticles
KW - Iron oxide nanoparticles
KW - Upconversion nanoparticles
PY - 2024
DO - https://doi.org/10.1007/s12274-024-6970-1
VL - 17
IS - 11
SP - 10119
EP - 10126
PB - Springer
AN - OPUS4-61459
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tavernaro, Isabella
A1 - Sander, P. C.
A1 - Andresen, Elina
A1 - Schedler, U.
A1 - Resch-Genger, Ute
T1 - Expanding the Toolbox of Simple, Cost-Efficient, and Automatable Methods for Quantifying Surface Functional Groups on Nanoparticles� Potentiometric Titration
N2 - Measuring surface functional groups (FGs) on nanomaterials (NMs) is essential for designing dispersible and stable NMs with tailored and predictable functionality. FG screening and quantification also plays a critical role for subsequent processing steps, NM long-term stability, quality control of NM production, and risk assessment studies and enables the implementation of sustainable and safe(r)-by-design concepts. This calls for simple and cost-efficient methods for broadly utilized FGs that can be ideally automated to speed up FG screening, monitoring, and quantification. To expand our NM surface analysis toolbox, focusing on simple methods and broadly available, cost-efficient instrumentation, we explored a NM-adapted pH titration method with potentiometric and optical readout for measuring the total number of (de)protonable FGs on representatively chosen commercial and custom-made aminated silica nanoparticles (SiO2 NPs). The accuracy and robustness of our stepwise optimized workflows was assessed by several operators in two laboratories and method validation was done by cross-comparison with two analytical methods relying on different signal generation principles. This included traceable, chemo-selective quantitative nuclear magnetic resonance spectroscopy (qNMR) and thermogravimetric analysis (TGA), providing the amounts of amino silanes released by particle dissolution and the total mass of the surface coatings. A comparison of the potentiometric titration results with the reporter-specific amounts of surface amino FGs determined with the previously automated fluorescamine (Fluram) assay highlights the importance of determining both quantities for surface-functionalized NMs. In the future, combined NM surface analysis with optical assays and pH titration will simplify quality control of NM production processes and stability studies and can yield large data sets for NM grouping that facilitates further developments in regulation and standardization.
KW - Quality assurance
KW - Fluorescence
KW - Nano
KW - Particle
KW - Synthesis
KW - Characterization
KW - Advanced material
KW - Surface
KW - Standardization
KW - Reference material
KW - Functional group
KW - Quantification
KW - Coating
KW - Automation
KW - Potentiometry
KW - Method
KW - Validation
KW - Optical assay
KW - Fluram
KW - Fluorescamine
KW - qNMR
KW - Comparison
KW - ILC
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642371
DO - https://doi.org/10.1021/acsmeasuresciau.5c00062
SN - 2694-250X
SP - 1
EP - 13
PB - American Chemical Society
CY - Washington, DC
AN - OPUS4-64237
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Herter, Sven-Oliver
A1 - Haase, Hajo
A1 - Koch, Matthias
T1 - Semisynthesis of Stable Isotope-Labeled Ergot Alkaloids for HPLC-MS/MS Analysis
N2 - Ergot alkaloids (EAs) are prevalent food contaminants affecting cereals, such as rye, wheat, and barley worldwide. To ensure EU safety standards, the six most common EAs: ergometrine, ergotamine, ergosine, ergocornine, ergocristine, and ergocryptine, and their epimers, are quantified using HPLC-MS/MS, as described in the European Standard Method EN 17425:2021. However, this can be challenging and time-consuming in food matrices without appropriate internal standards and highlights the need for more robust and precise analytical tools to support their monitoring. The development of isotope-labeled EAs directly addresses this gap, offering improved accuracy and leading to more consistency across laboratories and consequently to more consumer safety. Therefore, we developed a semisynthetic approach, building upon our previous work where native ergotamine was N6-demethylated to norergotamine and subsequently remethylated using iodomethane (13CD3-I). Herein, we are now able to present the successful synthesis of all of the isotopically labeled priority EAs. These isotope-labeled standards were tested against their native counterparts using HPLC coupled with HR-MS/MS. The chromatographic and mass spectrometric properties of the unlabeled and isotopically labeled EAs match exactly, confirming their successful synthesis and structure. These standards can now be utilized to enhance the accuracy and reliability of EA quantification in food and feed.
KW - Reference Material
KW - HPLC-MS/MS
KW - Mycotoxins
KW - Ergot Alkaloids
KW - Stable Isotope Dilution Analysis
KW - Semisynthesis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639692
DO - https://doi.org/10.1021/acs.jafc.5c03345
SN - 0021-8561
VL - 73
IS - 29
SP - 18412
EP - 18419
PB - American Chemical Society (ACS)
AN - OPUS4-63969
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stiegler, L. M. S.
A1 - Wegner, Karl David
A1 - Weigert, Florian
A1 - Peukert, W.
A1 - Resch-Genger, Ute
A1 - Walter, J.
T1 - Analysis of Giant-Shell CdSe/CdS Quantum Dots via Analytical Ultracentrifugation Combined with Spectrally Resolved Photoluminescence
N2 - Knowledge of the structure–property relationships of functional nanomaterials, including, for example, their size- and composition-dependent photoluminescence (PL) and particle-to-particle variations, is crucial for their design and reproducibility. Herein, the Angstrom-resolution capability of an analytical ultracentrifuge combined with an in-line multiwavelength emission detection system (MWE-AUC) for measuring the sedimentation coefficient-resolved spectrally corrected PL spectra of dispersed nanoparticles is demonstrated. The capabilities of this technique are shown for giant-shell CdSe/CdS quantum dots (g-QDs) with a PL quantum yield (PL QY) close to unity capped with oleic acid and oleylamine ligands. The MWE-AUC PL measurements are calibrated and validated with certified fluorescence standards. The spectrally corrected and size-dependent PL spectra of the g-QDs derived from a single MWE-AUC experiment are then analyzed and compared with the results of single-particle spectroscopic studies, yielding the PL spectra, decay kinetics, and blinking behavior of individual g-QDs. This study underlines the vast potential of MWE-AUC with in-line optical detection for the characterization of advanced nanomaterials with a complex structure.
KW - Quantum dots
KW - Analytical ultracentrifugation
KW - Photoluminescence
KW - Advanced nanomaterial characterization
KW - Calibrated fluorescence measurements
KW - Reference materials
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624357
DO - https://doi.org/10.1002/smtd.202401700
SN - 2366-9608
SP - 1
EP - 7
PB - Wiley VHC-Verlag
AN - OPUS4-62435
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Richter, Maria
A1 - Güttler, Arne
A1 - Pauli, Jutta
A1 - Vogel, K.
A1 - Homann, Christian
A1 - Würth, Christian
A1 - Resch-Genger, Ute
T1 - Extending certified spectral fluorescence standards for the calibration and performance validation of fluorescence instruments to the NIR—closing the gap from 750 to 940 nm with two novel NIR dyes
N2 - Fluorescence techniques such as fluorescence spectroscopy, microfluorometry, and fluorescence microscopy, providing spectral, intensity, polarization, and lifetime information, are amongst the most broadly utilized analytical methods in the life and materials sciences. However, the measured fluorescence data contain sample- and instrument-specific contributions, which hamper their comparability across instruments and laboratories. Comparable, instrument-independent fluorescence data require the determination of the fluorescence instrument’s wavelength-dependent spectral responsivity, also termed emission correction curve, for the same instrument settings as those used for the fluorescence measurements as a prerequisite for the subsequent correction of the measured instrument-specific data. Such a spectral correction is essential for the performance comparison of different fluorescent labels and reporters, quantitative fluorescence measurements, the determination of the fluorescence quantum yield, and the spectroscopic measure for the fluorescence efficiency of a fluorophore. Simple-to-use tools for obtaining emission correction curves are chromophore-based reference materials (RMs), referred to as fluorescence standards, with precisely known, preferably certified instrument-independent fluorescence spectra. However, for the increasingly used near-infrared (NIR) wavelength region >700 nm, at present, no spectral fluorescence standards are available. To close this gap, we developed two novel spectral fluorescence standards, BAM F007 and BAM-F009, with broad emission bands from about 580 to 940 nm in ethanolic solution. These liquid fluorescence standards currently under certification, which will be released in 2025, will expand the wavelength range of the already available certified Calibration Kit BAM F001b-F005b from about 300–730 to 940 nm. In this research article, we will detail the criteria utilized for dye and matrix selection and the homogeneity and stability tests accompanying dye certification as well as the calculation of the wavelength-dependent uncertainty budgets of the emission spectra BAM F007 and BAM-F009, determined with the traceably calibrated BAM reference spectrofluorometer. These fluorescence standards can provide the basis for comparable fluorescence measurements in the ultraviolet, visible, and NIR for the fluorescence community.
KW - Quality assurance
KW - Reference material
KW - Fluorescence
KW - Dye
KW - Traceability
KW - Metrology
KW - Calibration
KW - Reference data
KW - Reference product
KW - Digital certificate
KW - NIR
KW - Instrument performance validation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626317
DO - https://doi.org/10.1007/s00216-024-05723-w
SN - 1618-2650
SP - 1
EP - 15
PB - Springer
AN - OPUS4-62631
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Deumer, J.
A1 - Andresen, Elina
A1 - Gollwitzer, C.
A1 - Schürmann, R.
A1 - Resch-Genger, Ute
T1 - Adding More Shape to Nanoscale Reference Materials-LiYF4:Yb,Tm Bipyramids as Standards for Sizing Methods and Particle Number Concentration
N2 - The increasing industrial use of nanomaterials calls for the reliable characterization of their physicochemical key properties like size, size distribution, shape, and surface chemistry, and test and reference materials (RMs) with sizes and shapes, closely matching real-world nonspheric nano-objects. An efficient strategy to minimize efforts in producing nanoscale RMs (nanoRMs) for establishing, validating, and standardizing methods for characterizing nanomaterials are multimethod nanoRMs.
Ideal candidates are lanthanide-based, multicolor luminescent, and chemically inert nanoparticles (NPs) like upconversion nanoparticles (UCNPs), which can be prepared in different sizes, shapes, and chemical composition with various surface coatings. This makes UCNPs interesting candidates as standards not only for sizing methods, but also for element-analytical methods like laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS), quantitative bioimaging methods like X-ray fluorescence computed tomography (XFCT), and luminescence methods and correlative measurements.
Here, we explore the potential of two monodisperse LiYF4:Yb,Tm bipyramids with peak-to-peak distances of (43 ± 2) nm and (29 ± 2) nm as size standards for small-angle X-ray scattering (SAXS) and tools for establishing and validating the sophisticated simulations required for the analysis of SAXS data derived from dispersions of nonspheric nano-objects. These SAXS studies are supplemented by two-dimensional (2D)-transmission electron microscopy measurements of the UCNP bipyramids. Additionally, the particle number concentration of cyclohexane dispersions of these UCNP bipyramids is determined by absolute SAXS measurements, complemented by gravimetry, thermogravimetric analysis (TGA), and inductively coupled plasma optical emission spectrometry (ICP-OES). This approach enables traceable particle number concentration measurements of ligand-capped nonspheric particles with unknown chemical composition.
KW - Fluorescence
KW - Upconversion nanoparticles
KW - SAXS
KW - Particle number concentration
KW - Reference material
KW - Traceability
KW - Quality assurance
KW - Quantum yield
KW - Spectroscopy
KW - Synthesis
KW - Quantification
KW - NanoRM
KW - Nano
KW - Particle
KW - Bipyramid
KW - Reference data
KW - Simulation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-617940
DO - https://doi.org/10.1021/acs.analchem.4c03641
SP - 1
EP - 8
PB - ACS Publications
AN - OPUS4-61794
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Knoche, Lisa
A1 - Lisec, Jan
A1 - Schwerdtle, T.
A1 - Koch, Matthias
T1 - LC-HRMS-Based Identification of Transformation Products of the Drug Salinomycin Generated by Electrochemistry and Liver Microsome
N2 - The drug salinomycin (SAL) is a polyether antibiotic and used in veterinary Medicine as coccidiostat and growth promoter. Recently, SAL was suggested as a potential anticancer drug.
However, transformation products (TPs) resulting from metabolic and environmental degradation of SAL are incompletely known and structural information is missing. In this study, we therefore systematically investigated the formation and identification of SAL derived TPs using electrochemistry (EC) in an electrochemical reactor and rat and human liver microsome incubation (RLM and HLM) as TP generating methods. Liquid chromatography (LC) coupled to high-resolution mass spectrometry (HRMS) was applied to determine accurate masses in a suspected target analysis to identify TPs and to deduce occurring modification reactions of derived TPs. A total of 14 new, structurally different TPs were found (two EC-TPs, five RLM-TPs, and 11 HLM-TPs). The main modification reactions are decarbonylation for EC-TPs and oxidation (hydroxylation) for RLM/HLM-TPs. Of particular interest are potassium-based TPs identified after liver microsome incubation because these might have been overlooked or declared as oxidated sodium adducts in previous, non-HRMS-based studies due to the small mass difference between K and O + Na of 21 mDa. The MS fragmentation pattern of TPs was used to predict the position of identified modifications in the SAL molecule. The obtained knowledge regarding transformation reactions and novel TPs of SAL will contribute to elucidate SAL-metabolites with regards to structural prediction.
KW - Salinomycin
KW - Ionophore antibiotics
KW - Transformation product
KW - Electrochemistry
KW - Rat/human liver microsomes
KW - HRMS
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542543
DO - https://doi.org/10.3390/antibiotics11020155
SN - 2079-6382
VL - 11
IS - 2
SP - 155
PB - MDPI
CY - Basel
AN - OPUS4-54254
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kuner, Maximilian
A1 - Lisec, Jan
A1 - Picher, Marie-Idrissa
A1 - Rigo, Massimo
A1 - Konetzki, Jörg
A1 - Haase, Hajo
A1 - Koch, Matthias
T1 - Development and Application of Isotope Labelled Internal Standards in a Sum Parameter Method for Ergot Alkaloid Screening of Food
N2 - Ergot alkaloids are a group of toxic compounds, formed by fungi on infested grasses. In 2022, the European Commission set into effect maximum levels for the sum of the twelve major ergot alkaloids in multiple foods. To facilitate the laborious and costly individual quantification of the twelve major ergot alkaloids by HPLC–MS/MS or -FLD, we recently reported a sum parameter method (SPM) for ergot alkaloid quantification. Here, derivatization to lysergic acid hydrazide—a derivative of the mutual ergoline backbone in all ergot alkaloids—allowed simplified determination of all ergot alkaloids in flour via HPLC-FLD. For the measurement of more complex matrices like processed foods, we now developed a MS/MS-based SPM. Two internal standards (IS), isotopically labelled at different positions of the molecule, were synthesized and employed in the MS/MS-measurements. Method performance using either the 13CD3-labelled or the 15N2-labelled IS was evaluated on naturally contaminated rye and wheat flour samples as well as on processed food matrices. Employing the 13CD3-labelled IS leads to lower variances and better consistency with the reference data (obtained by the FLD-based SPM) in flour samples compared to the 15N2-labelled IS. The novel method significantly improves the measurement of ergot alkaloids in complex food matrices, due to their increased selectivity and thus lower interferences. Furthermore, the application of isotope labelled IS obviates the need for time-consuming steps like the determination of recovery rate based, matrix specific correction factors as described in the MS/MS-based European standard method for ergot alkaloid quantification (EN 17425).
KW - Mycotoxins
KW - Sum Parameter Method
KW - Isotope Labelling
KW - HPLC-MS/MS
KW - Analytical Chemistry
KW - Lysergic acid hydrazide
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588582
DO - https://doi.org/10.1007/s12161-023-02553-x
SN - 1936-976X
VL - 17
IS - 1
SP - 119
EP - 128
PB - Springer
CY - New York, NY
AN - OPUS4-58858
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scholtz, Lena
A1 - Eckert, J. G.
A1 - Graf, Rebecca T.
A1 - Kunst, A.
A1 - Wegner, Karl David
A1 - Bigall, N. C.
A1 - Resch-Genger, Ute
T1 - Correlating semiconductor nanoparticle architecture and applicability for the controlled encoding of luminescent polymer microparticles
N2 - Luminophore stained micro- and nanobeads made from organic polymers like polystyrene (PS) are broadly used in the life and material sciences as luminescent reporters, for bead-based assays, sensor arrays, printable barcodes, security inks, and the calibration of fluorescence microscopes and flow cytometers. Initially mostly prepared with organic dyes, meanwhile luminescent core/shell nanoparticles (NPs) like spherical semiconductor quantum dots (QDs) are increasingly employed for bead encoding. This is related to their narrower emission spectra, tuneability of emission color, broad wavelength excitability, and better photostability. However, correlations between particle architecture, morphology, and photoluminescence (PL) of the luminescent nanocrystals used for encoding and the optical properties of the NP-stained beads have been rarely explored. This encouraged us to perform a screening study on the incorporation of different types of luminescent core/shell semiconductor nanocrystals into polymer microparticles (PMPs) by a radical-induced polymerization reaction. Nanocrystals explored include CdSe/CdS QDs of varying CdS shell thickness, a CdSe/ZnS core/shell QD, CdSe/CdS quantum rods (QRs), and CdSe/CdS nanoplatelets (NPLs).
Thereby, we focused on the applicability of these NPs for the polymerization synthesis approach used and quantified the preservation of the initial NP luminescence. The spectroscopic characterization of the resulting PMPs revealed the successful staining of the PMPs with luminescent CdSe/CdS QDs and CdSe/CdS NPLs. In contrast, usage of CdSe/CdS QRs and CdSe QDs with a ZnS shell did not yield luminescent PMPs. The results of this study provide new insights into structure–property relationships between NP stained PMPs and the initial luminescent NPs applied for staining and underline the importance of such studies for the performance optimization of NP-stained beads.
KW - Quantitative spectroscopy
KW - Energy transfer
KW - Synthesis
KW - Surface chemistry
KW - Semiconductor quantum dot
KW - Luminescence
KW - Nano
KW - Particle
KW - Quantum yield
KW - Lifetime
KW - Quality assurance
KW - Polymer particle
KW - Quantum rod
KW - Nanoplatelet
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602206
DO - https://doi.org/10.1038/s41598-024-62591-1
SN - 2045-2322
VL - 14
SP - 1
EP - 16
AN - OPUS4-60220
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Frenzel, F.
A1 - Fiedler, S.
A1 - Bardan, A.
A1 - Güttler, Arne
A1 - Würth, Christian
A1 - Resch-Genger, Ute
T1 - Influence of Measurement Geometry and Blank on Absolute Measurements of Photoluminescence Quantum Yields of Scattering Luminescent Films
N2 - For a series of 500 μm-thick polyurethane films containing different concentrations of luminescent and scattering YAG:Ce microparticles, we systematically explored and quantified pitfalls of absolute measurements of photoluminescence quantum yields (Φf) for often employed integrating sphere (IS) geometries, where the sample is placed either on a sample holder at the bottom of the IS surface or mounted in the IS center. Thereby, the influence of detection and illumination geometry and sample position was examined using blanks with various scattering properties for measuring the number of photons absorbed by the sample. Our results reveal that (i) setup configurations where the scattering sample is mounted in the IS center and (ii) transparent blanks can introduce systematic errors in absolute Φf measurements.
For strongly scattering, luminescent samples, this can result in either an under- or overestimation of the absorbed photon flux and hence an under- or overestimation of Φf. The size of these uncertainties depends on the scattering properties of the sample and instrument parameters, such as sample position, IS size, wavelength-dependent reflectivity of the IS surface coating, and port configuration. For accurate and reliable absolute Φf measurements, we recommend (i) a blank with scattering properties closely matching those of the sample to realize similar distributions of the diffusely scattered excitation photons within the IS, and (ii) a sufficiently high sample absorption at the excitation wavelength. For IS setups with center-mounted samples, measurement geometries should be utilized that prevent the loss of excitation photons by reflections from the sample out of the IS.
KW - Quality assurance
KW - Fluorescence
KW - Nano
KW - Particle
KW - Quantum yield
KW - Characterization
KW - Silica
KW - Scattering
KW - Uncertainty
KW - Film
KW - Pphosphor
KW - YAG:Ce
KW - LED
KW - Converter material
KW - Solid material
KW - Polymer
KW - Composite material
KW - Advanced material
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638304
DO - https://doi.org/10.1021/acs.analchem.4c06726
SN - 1520-6882
SP - 1
EP - 8
PB - ACS Publications
AN - OPUS4-63830
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kuner, Maximilian
A1 - Lisec, Jan
A1 - Mauch, Tatjana
A1 - Konetzki, J.
A1 - Haase, H.
A1 - Koch, Matthias
T1 - Quantification of Ergot Alkaloids via Lysergic Acid Hydrazide—Development and Comparison of a Sum Parameter Screening Method
N2 - Ergot alkaloids are a group of mycotoxins occurring in products derived from various grasses (e.g., rye) and have been regulated in the EU recently. The new maximum levels refer to the sum of the six most common ergot alkaloids in their two stereoisomeric forms in different food matrices. Typically, these twelve compounds are individually quantified via HPLC-MS/MS or -FLD and subsequently summed up to evaluate food safety in a time-consuming process. Since all these structures share the same ergoline backbone, we developed a novel sum parameter method (SPM) targeting all ergot alkaloids simultaneously via lysergic acid hydrazide. After extraction and clean-up, in analogy to the current European standard method EN 17425 (ESM) for ergot alkaloid quantitation, the samples were derivatized by an optimized hydrazinolysis protocol, which allowed quantitative conversion after 20 min at 100 °C. The new SPM was evaluated against another established HPLC-FLD-based method (LFGB) and the HPLC-MS/MS-based ESM using six naturally contaminated rye and wheat matrix reference materials. While the SPM provided comparable values to the ESM, LFGB showed deviating results. Determined recovery rates, limits of detection and quantification of all three employed methods confirm that the new SPM is a promising alternative to the classical approaches for ergot alkaloid screening in food.
KW - Ergot alkaloids
KW - Sum Parameter
KW - Mycotoxins
KW - Derivatization
KW - Hydrazinolysis
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573968
DO - https://doi.org/10.3390/molecules28093701
SN - 0015-2684
VL - 28
IS - 9
SP - 3701
PB - MDPI
CY - Basel
AN - OPUS4-57396
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Li, X.M.
A1 - Li, H.M.
A1 - Zhang, Q.H.
A1 - Lu, X.H.
A1 - Li, S.Q.
A1 - Koch, Matthias
A1 - Polzer, J.
A1 - Hackenber, R.
A1 - Moniruzzaman, M.
A1 - Khan, M.
A1 - Kakoulides, E.
A1 - Pak-Wing, K.
A1 - Richy,
A1 - Chi-Shing, N.
A1 - Lu, T.
A1 - Gui, E.M.
A1 - Cheow, P.S.
A1 - Teo, T.L.
A1 - Rego, E.
A1 - Garrido, B.
A1 - Carvalho, L.
A1 - Leal, R.
A1 - Violante, F.
A1 - Baek, S.Y.
A1 - Lee, S.
A1 - Choi, K.
A1 - Kim, B.
A1 - Bucar-Miklavcic, M.
A1 - Hopley, C.
A1 - Nammoonnoy, J.
A1 - Murray, J.
A1 - Wilson, W.
A1 - Toman, B.
A1 - Itoh, N.
A1 - Gokcen, T.
A1 - Krylov, A.
A1 - Mikheeva, A.
T1 - CCQM-K146 low-polarity analyte in high fat food: benzo a pyrene in olive oil
N2 - The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix.
KW - Metrology
KW - CCQM
KW - Food
KW - PAH
PY - 2020
DO - https://doi.org/10.1088/0026-1394/57/1a/08017
VL - 57
IS - 1a
SP - 08017
AN - OPUS4-52435
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hoffmann, A.
A1 - Lischeid, G.
A1 - Koch, Matthias
A1 - Lentzsch, P.
A1 - Sommerfeld, Thomas
A1 - Müller, M.H.
T1 - Co-Cultivation of Fusarium, Alternaria, and Pseudomonas on Wheat-Ears Affects Microbial Growth and Mycotoxin Production
N2 - Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads.
Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria enuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9).
Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies.
KW - Antagonists
KW - Microbe interactions
KW - Mycotoxins
KW - Priority effect
KW - SOM-SM
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521554
DO - https://doi.org/10.3390/microorganisms9020443
VL - 9
IS - 2
SP - 443
PB - MDPI
AN - OPUS4-52155
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rezvani, A.
A1 - Wang, Z.
A1 - Wegner, Karl David
A1 - Soltanmoradi, H.
A1 - Kichigin, A.
A1 - Zhou, X.
A1 - Gantenberg, T.
A1 - Schram, J.
A1 - Zubiri, B. A.
A1 - Spiecker, E.
A1 - Walter, J.
A1 - Resch-Genger, Ute
A1 - Segets, D.
T1 - Separation of Indium Phosphide/Zinc Sulfide Core−Shell Quantum Dots from Shelling Byproducts through Multistep Agglomeration
N2 - Semiconductor quantum dots (QDs) possess unique electronic and optical properties, making them promising candidates for applications in lightemitting diodes, solar cells, bioimaging, and photocatalysis. Precise control over their size, shape, and chemical and electronic structure is crucial to ensure the desired functional properties and optimize device performance. However, challenges in QD synthesis and post-synthesis modification persist, especially in large-scale production. This study addresses the classification of QDs synthesized in a tubular flow reactor consisting of a mixture of the desired InP/ZnS core−shell QDs and QDs made from the shell material, i.e., here ZnS QDs formed as a byproduct during the formation step of the ZnS shell. The homogeneous nucleation of ZnS nanoparticles from the shelling material introduces a heterogeneity in size and composition and affects the optical properties of the resulting QDs. To address this issue, we developed a size-selective agglomeration (SSA) technique by incrementally introducing ethanol as a poor solvent and classified the synthesized QDs into 13 distinct fractions. These 13 fractions are sorted into three distinct groups: (i) larger InP/ZnS QDs, (ii) a combination of smaller InP/ZnS QDs and larger ZnS QDs, and (iii) predominant ZnS QDs with some very tiny InP/ZnS QDs. The comprehensive characterization of the fractions was conducted using UV−visible absorption spectroscopy, photoluminescence spectroscopy, high-resolution scanning transmission electron microscopy, energy-dispersive X-ray spectroscopy, total reflection X-ray fluorescence, and analytical ultracentrifugation. We could demonstrate that our method effectively separated unwanted ZnS QDs from the target InP/ZnS QDs. In addition, the fractions enriched in smaller InP/ZnS QDs exhibited a higher photoluminescence quantum yield compared to the fractions with larger QDs. This demonstrates the efficacy of SSA in finetuning the composition of QD mixtures produced on a larger scale to improve their functional properties. This approach provides fundamental understanding toward the development of a scalable two-dimensional classification process for such ultrasmall nanoparticles by particle size and composition.
KW - Quality assurance
KW - Reference material
KW - Nano
KW - Particle
KW - Quantum dot
KW - Synthesis
KW - Flow reactor
KW - InP
KW - Shell
KW - ZnS
KW - Surface chemistry
KW - Method
KW - Fluorescence
KW - Quantum yield
KW - TEM
PY - 2025
DO - https://doi.org/10.1021/acsnano.4c18530
SN - 1936-086X
VL - 19
IS - 20
SP - 19080
EP - 19094
PB - ACS Publications
AN - OPUS4-63215
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Riedel, Juliane
A1 - Recknagel, Sebastian
A1 - Sassenroth, Diana
A1 - Mauch, Tatjana
A1 - Buttler, Sabine
A1 - Sommerfeld, Thomas
A1 - Penk, Sibylle
A1 - Koch, Matthias
T1 - Development and certification of a reference material for zearalenone in maize germ oil
N2 - Zearalenone (ZEN), an estrogenic mycotoxin produced by several species of Fusarium fungi, is a common contaminant of cereal-based food worldwide. Due to frequent occurrences associated with high levels of ZEN, maize oil is a particular source of exposure. Although a European maximumlevel for ZEN in maize oil exists according to Commission Regulation (EC) No. 1126/2007 along with a newly developed international standard method for analysis, certified reference materials (CRM) are still not available. To overcome this lack, the first CRM for the determination of ZEN in contaminated maize germ oil (ERM®-BC715) was developed in the frame of a European Reference Materials (ERM®) project according to the requirements of ISO Guide 35. The whole process of CRM development including preparation, homogeneity and stability studies, and value assignment is presented. The assignment of the certified mass fraction was based upon an in-house study using high-performance liquid chromatography isotope dilution tandem mass spectrometry. Simultaneously, to support the in-house certification study, an interlaboratory comparison study was conducted with 13 expert laboratories using different analytical methods. The certified mass fraction and expanded uncertainty (k=2) of ERM®-BC715 (362± 22) μg kg−1 ZEN are traceable to the SI. This reference material is intended for analytical quality control and contributes to the improvement of consumer protection and food safety.
KW - Fusarium mycotoxin
KW - Vegetable edible oil
KW - Food analysis
KW - European Reference Material
KW - Quality assurance
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531831
DO - https://doi.org/10.1007/s00216-021-03532-z
SN - 1618-2642
SN - 1618-2650
VL - 413
IS - 21
SP - 5483
EP - 5491
PB - Springer
CY - Berlin
AN - OPUS4-53183
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kuner, Maximilian
A1 - Kühn, S.
A1 - Haase, H.
A1 - Meyer, Klas
A1 - Koch, Matthias
T1 - Cleaving Ergot Alkaloids by Hydrazinolysis - A Promising Approach for a Sum Parameter Screening Method
N2 - Ergot alkaloids are mycotoxins formed by fungi of the Claviceps genus, which are some of the most common contaminants of food and feed worldwide. These toxins are a structurally heterogeneous group of compounds, sharing an ergoline backbone. Six structures and their corresponding stereoisomers are typically quantified by either HPLC-FLD or HPLC-MS/MS and the values subsequently summed up to determine the total ergot alkaloid content. For the development of a screening method targeting all ergot alkaloids simultaneously, the alkaloids need to be transferred to one homogeneous structure: a lysergic acid derivative. In this study, two promising cleaving methods—acidic esterification and hydrazinolysis—are compared, using dihydroergocristine as a model compound. While the acidic esterification proved to be unsuitable, due to long reaction times and oxidation sensitivity, hydrazinolysis reached a quantitative yield in 40-60 min. Parallel workup of several samples is possible. An increasing effect on the reaction rate by the addition of ammonium iodide was demonstrated. Application of hydrazinolysis to a major ergot alkaloid mix solution showed that all ergopeptines were cleaved, but ergometrine/-inine was barely affected. Still, hydrazinolysis is a suitable tool for the development of a sum parameter screening method for ergot alkaloids in food and feed.
KW - Ergot alkaloids
KW - Sum parameter method
KW - Hydrazinolysis
KW - Esterification
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527508
DO - https://doi.org/10.3390/toxins13050342
VL - 13
IS - 5
SP - 342
PB - MDPI
CY - Basel, Switzerland
AN - OPUS4-52750
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wasternack, J.
A1 - Schröder, H. V.
A1 - Witte, J. F.
A1 - Ilisson, M.
A1 - Hupatz, H.
A1 - Hille, J. F.
A1 - Gaedke, M.
A1 - Valkonen, A. M.
A1 - Sobottka, S.
A1 - Krappe, A.
A1 - Schubert, M.
A1 - Paulus, B.
A1 - Rissanen, K.
A1 - Sarkar, B.
A1 - Eigler, S.
A1 - Resch-Genger, Ute
A1 - Schalley, C. A.
T1 - Switchable protection and exposure of a sensitive squaraine dye within a redox active rotaxane
N2 - In nature,molecular environments in proteins can sterically protect and stabilize reactive species such as organic radicals through non-covalent interactions.Here, wereport a near-infrared fluorescent rotaxane in which the stabilization of a chemically labile squaraine fluorophore by the coordination of a tetralactam macrocycle can be controlled chemically and electrochemically. The rotaxane can be switched between two co-conformations inwhich thewheel either stabilizes or exposes the fluorophore. Coordination by the wheel affects the squaraine’s stability across four redox states and renders the radical anion significantly more stable—by a factor of 6.7—than without protection by a mechanically bonded wheel. Furthermore, the fluorescence properties can be tuned by the redox reactions in a stepwise manner. Mechanically interlockedmolecules provide an excellent scaffold to stabilize and selectively expose reactive species in a co-conformational switching process controlled by external stimuli.
KW - Fluorescence
KW - Dye
KW - Sensor
KW - Quantum yield
KW - Spectroscopy
KW - Photophysics
KW - Synthesis
KW - Squaraine
KW - Switch
KW - Redox-active
KW - Rotaxane
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614959
DO - https://doi.org/10.1038/s42004-024-01312-1
VL - 7
SP - 1
EP - 11
AN - OPUS4-61495
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Andreato, E.
A1 - Panov, N.
A1 - Artiga, A.
A1 - Osipova, Viktoriia
A1 - Resch-Genger, Ute
A1 - Ximendes, E.
A1 - Molina, P.
A1 - Canton, P.
A1 - Marin, R.
T1 - Indium-Based Fluoride Nanoparticles Doped with Chromium for Near-Infrared Luminescence
N2 - Transition metal (TM) and rare earth (RE) ion-doped nanoparticles (NPs) are photoluminescent materials of technological relevance in bioimaging, sensing, and light conversion. Fluoride NPs are particularly attractive in this context, since they combine low-energy phonons, high chemical stability, optical transparency, size, and architecture tunability. Yet, nearly all reported colloidal fluoride NPs (e.g., NaYF4 and LiYF4) can only be efficiently doped with RE3+ and not with luminescent TM ions. Herein, we contribute to filling this gap in materials science by reporting Na3InF6 NPs doped with Cr3+ as a model luminescent TM ion. We unveil the heat-driven NP formation mechanism, which involves a cubic-to-monoclinic phase conversion, similarly to the cubic-tohexagonal phase conversion in NaYF4. Reaction temperatures above 225 °C and reaction time have a limited impact on the NP morphology, while the amount of fluoride precursor and oleylamine grants control over the NP size. After verifying that Na3InF6 NPs show negligible cytotoxicity toward U-87 cell line, we study the optical properties of these NPs upon Cr3+ doping.
Temperature-dependent photoluminescence measurements indicate that Cr3+ ions experience a weak crystal field in the Na3InF6 host lattice, while their photoluminescence lifetime varies linearly in the 20−50 °C range. These results set the ground for further studies of photoluminescent TM-doped fluoride NPs, toward their applications in bioimaging, sensing, and light-converting devices.
KW - Quality assurance
KW - Fluorescence
KW - Traceability
KW - Nano
KW - Particle
KW - Synthesis
KW - Quantum yield
KW - NIR
KW - Mechanism
KW - Characterization
KW - XRD
KW - Phase transition
KW - Ligand
KW - Surface
KW - Doping
KW - Lifetime
PY - 2025
DO - https://doi.org/10.1021/acs.chemmater.4c03335
SN - 1520-5002
SP - 1
EP - 14
PB - American Chemical Society
AN - OPUS4-63073
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lozano-Martín, Daniel
A1 - Tuma, Dirk
A1 - Chamorro, César R.
T1 - Evaluation of Reference Equations of State for Density Prediction in Regasified LNG Mixtures Using High-Precision Experimental Data
N2 - This study evaluates the performance of three reference equations of state (EoS), AGA8-DC92, GERG-2008, and SGERG-88, in predicting the density of regasified liquefied natural gas (RLNG) mixtures. A synthetic nine-component RLNG mixture was gravimetrically prepared. High-precision density measurements were obtained using a single-sinker magnetic suspension densimeter over a temperature range of (250 to 350) K and pressures up to 20 MPa. The experimental data were compared with EoS predictions to evaluate their accuracy. AGA8-DC92 and GERG-2008 showed excellent agreement with the experimental data, with deviations within their stated uncertainty. In contrast, SGERG-88 exhibited significantly larger deviations for this RLNG mixture, particularly at low temperatures of (250 to 260) K, where discrepancies reached up to 3 %. Even at 300 K, deviations larger than 0.4 % were observed at high pressures, within the model’s uncertainty, but notably higher than those of the other two EoSs. The analysis was extended to three conventional 11-component natural gas mixtures (labeled G420 NG, G431 NG, and G432 NG), previously studied by our group using the same methodology. While SGERG-88 showed reduced accuracy for the RLNG mixture, it performed reasonably well for these three mixtures, despite two of them have a very similar composition to the RLNG. This discrepancy is attributed to the lower CO2 and N2 content typical in RLNG mixtures, demonstrating the sensitivity of EoS performance to minor differences in composition. These findings highlight the importance of selecting appropriate EoS models for accurate density prediction in RLNG applications.
KW - Regasified LNG
KW - Equation of state
KW - Density
KW - Gravimetric preparation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646506
DO - https://doi.org/10.1007/s10765-025-03669-4
SN - 0195-928X
VL - 46
SP - 1
EP - 25
PB - Springer Science and Business Media LLC
CY - Heidelberg
AN - OPUS4-64650
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Boyraz, B.
A1 - Saatz, Jessica
A1 - Pompös, I.-M.
A1 - Gad, Michel
A1 - Dernedde, J.
A1 - Maier, A.-M. B.
A1 - Moscovitz, O.
A1 - Seeberger, P. H.
A1 - Traub, Heike
A1 - Tauber, R.
T1 - Imaging Keratan Sulfate in Ocular Tissue Sections by Immunofluorescence Microscopy and LA-ICP-MS
N2 - Carbohydrate-specific antibodies can serve as valuable tools to monitor alterations in the extracellular matrix resulting from pathologies. Here, the keratan sulfate-specific monoclonal antibody MZ15 was characterized in more detail by immunofluorescence microscopy as well as laser ablation ICP-MS using tissue cryosections and paraffin-embedded samples. Pretreatment with keratanase II prevented staining of samples and therefore demonstrated efficient enzymatic keratan sulfate degradation. Random fluorescent labeling and site-directed introduction of a metal cage into MZ15 were successful and allowed for a highly sensitive detection of the keratan sulfate landscape in the corneal stroma from rats and human tissue.
KW - Laser ablation
KW - Imaging
KW - Glycosaminoglycan
KW - ICP-MS
KW - Immunohistochemistry
KW - Immunofluorescence
KW - Tissue
PY - 2022
DO - https://doi.org/10.1021/acsabm.1c01240
VL - 5
IS - 2
SP - 853
EP - 861
PB - American Chemical Society
CY - Washington
AN - OPUS4-54341
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tjaden, B.
A1 - Lisec, Jan
A1 - Schramm, A.
T1 - N-Myc-induced metabolic rewiring creates novel therapeutic vulnerabilities in neuroblastoma
N2 - N-Myc is a transcription factor that is aberrantly expressed in many tumor types and is often correlated with poor patient prognosis. Recently, several lines of evidence pointed to the fact that oncogenic activation of Myc family proteins is concomitant with reprogramming of tumor cells to cope with an enhanced need for metabolites during cell growth. These adaptions are driven by the ability of Myc proteins to act as transcriptional amplifiers in a tissue-of-origin specific manner. Here, we describe the effects of N-Myc overexpression on metabolic reprogramming in neuroblastoma cells. Ectopic expression of N-Myc induced a glycolytic switch that was concomitant with enhanced sensitivity towards 2-deoxyglucose, an inhibitor of glycolysis. Moreover, global metabolic profiling revealed extensive alterations in the cellular metabolome resulting from overexpression of N-Myc. Limited supply with either of the two main carbon sources, glucose or glutamine, resulted in distinct shifts in steady-state metabolite levels and significant changes in glutathione metabolism. Interestingly, interference with glutamine-glutamate conversion preferentially blocked proliferation of N-Myc overexpressing cells, when glutamine levels were reduced. Thus, our study uncovered N-Myc induction and nutrient levels as important metabolic master switches in neuroblastoma cells and identified critical nodes that restrict tumor cell proliferation.
KW - Mass-Spectrometry
KW - Cancer
KW - MYCN
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507193
DO - https://doi.org/10.1038/s41598-020-64040-1
VL - 10
IS - 1
SP - 7157
AN - OPUS4-50719
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Smeir, E.
A1 - Leberer, S.
A1 - Blumrich, A.
A1 - Vogler, G.
A1 - Vasiliades, A.
A1 - Dresen, S.
A1 - Jaeger, Carsten
A1 - Gloaguen, Y.
A1 - Klose, C.
A1 - Beule, D.
A1 - Schulze, P.
A1 - Bodmer, R.
A1 - Foryst-Ludwig, A.
A1 - Kintscher, U.
T1 - Depletion of Cardiac Cardiolipin Synthase Alters Systolic and Diastolic Function
N2 - Cardiolipin (CL) is a major cardiac mitochondrial phospholipid maintaining regular mitochondrial morphology and function in cardiomyocytes. Cardiac CL production includes ist biosynthesis and a CL-remodeling process. Here we studied the impact of CL-biosynthesis and the enzyme Cardiolipin Synthase (CLS) on cardiac function.
CLS and cardiac CL-species were significantly downregulated in cardiomyocytes following catecholamine-induced cardiac damage in mice, accompanied by increased oxygen consumption rates, signs of oxidative stress and mitochondrial uncoupling. RNAi-mediated cardiomyocyte-specific knockdown of CLS in Drosophila melanogaster resulted in marked cardiac dilatation, severe impairment of systolic performance and slower diastolic filling velocity assessed by fluorescence-based heart imaging. Finally, we showed that CL72:8 is significantly decreased in cardiac samples from patients with heart failure with reduced ejection fraction (HFrEF). In summary, we identified CLS as a regulator of cardiac function. Considering the cardiac depletion of CL-species in HFrEF, pharmacological targeting of CLS may be a promising therapeutic approach.zeige mehrzeige weniger
KW - High-resolution mass spectrometry
KW - Nontarget analysis
KW - Heart failure
KW - Cardiolipins
KW - Lipidomics
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536833
DO - https://doi.org/10.1016/j.isci.2021.103314
VL - 24
IS - 11
SP - 103314
PB - Cell Press
AN - OPUS4-53683
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dalichow, Dirk
A1 - Blaschke, Jil
A1 - Wilsch, Gerd
A1 - Völker, Tobias
T1 - Revolutionizing Concrete Analysis and Maintenance with Laser-Induced Breakdown Spectroscopy
N2 - Laser-induced breakdown spectroscopy (LIBS) is a valuable complement to established methods for the chemical analysis of concrete. Compared to conventional techniques, LIBS enables spatially resolved imaging of harmful ion distributions within the cementitious matrix. It allows the simultaneous detection of all relevant ions and degradation mechanisms, facilitating a better understanding of interacting processes. The benefits of multi-element analysis are illustrated through selected examples that highlight the method’s superior information content. Ion penetration profiles are recorded at a resolution of 0.25 mm, providing high-quality input data for service life modelling. Instead of drill dust, a 50 mm core sample is used. The measurement is automated, requires no chemical reagents or elaborate sample preparation, and is completed within minutes.
KW - LIBS
KW - Durability
KW - Ion transport profiling
KW - Concrete analysis
KW - Service life assessment
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642846
DO - https://doi.org/10.58286/31656
SN - 1435-4934
VL - 30
IS - 10
SP - 1
EP - 8
PB - NDT.net GmbH & Co. KG
AN - OPUS4-64284
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heide, Maximilian
A1 - Reifenrath, Jonas
A1 - Herrmann, Alexander
A1 - Engelhard, Carsten
T1 - Fast and Sustainable Active Pharmaceutical Ingredient (API) Screening in Over-the-Counter and Prescription Drug Products by Surface-Assisted Plasma-Based Desorption/Ionization High-Resolution Mass Spectrometry
N2 - Fast chemical analysis of pharmaceutical preparations is important for quality assurance, counterfeit drug detection, and consumer health. While quantitative methods such as high-performance liquid chromatography mass spectrometry (HPLC-MS) are powerful, there is a need for sustainable and environmentally friendly methods, which require less chemicals and produce less waste. Here, solvent-free ambient desorption/ionization (ADI) MS methods are attractive because they do not require time-consuming chromatography, produce little to no chemical waste, and, thus, contribute to green chemistry practice. In addition, sample throughput can be higher compared to HPLC-MS. In this study, a method for direct analysis of single- and multi agent drugs using a plasma-based ADI source (flowing atmospheric-pressure afterglow, FAPA) coupled to high-resolution (HR) MS was developed and optimized for best performance. The approach is rapid and only requires analytes to be in solution (only a few µL) before application onto thin-layer chromatography (TLC) surfaces, specifically dimethyl (RP2-) and cyano (CN-) modified silica, for surface-assisted (SA) FAPA-HRMS measurements. No chromatographic separation was required, and the TLC plates served only as sample carriers. A broad variety of 19 active pharmaceutical ingredients (APIs) was carefully selected to cover analgesics, anesthetics, antibiotics, antiepileptics, calcium channel blockers, diuretics, expectorants, opioids, peripheral vasodilators, stimulants, and sympathomimetics. Fast screening and identification of APIs was performed by SA-FAPA-HRMS. Typically, the protonated molecular ion ([M+H]+) was the most abundant species, while some compounds (codeine, metamizole, phenoxymethylpenicillin, and torasemide) did show some degree of fragmentation. As a proof-of-principle application, benzocaine was directly detected in saliva samples post-intake of a lozenge. Time-resolved semi-quantitative screening was performed. The limit of detection for benzocaine in saliva was 8 ng/mL (48.4 fmol) using internal standard calibration and CN-HPTLC plates. In addition, direct quantification of artificially spiked saliva was performed with minimal sample preparation. Here, SA-FAPA-HRMS with a CN-HPTLC sample substrate yielded best performance (20.02±0.52 µg/mL, RSD=2.6%, deviation of -1.9% from the theoretical value) compared to RP2-TLC (18.97±1.37 µg/mL, RSD=7.2%, -7.0%), and HPLC-UV (18.51±0.03 µg/mL, RSD=0.2%, -9.3%) results. In conclusion, SA FAPA HRMS is considered attractive for rapid and sustainable analysis of pharmaceuticals with potential in non-invasive patient monitoring.
KW - Mass Spectrometry
KW - Pharmaceuticals
KW - Green Chemistry
KW - Ambient Desorption/Ionization
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640718
DO - https://doi.org/10.1039/D5AY01050K
SN - 1759-9660
VL - 17
IS - 18
SP - 7799
EP - 7809
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64071
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pisonero, J.
A1 - Traub, Heike
A1 - Cappella, Brunero
A1 - Álvarez-Llamas, C.
A1 - Méndez, A.
A1 - Richter, Silke
A1 - Ruiz Encinar, J.
A1 - Costa-Fernandez, J. M.
A1 - Bordel, N.
T1 - Exploring quantitative cellular biomaging and assessment of CdSe/ZnS quantum dots cellular uptake in single cells, using ns-LA-ICP-SFMS
N2 - High spatially resolved quantitative bioimaging of CdSe/ZnS Quantum Dots uptake in two kinds of cells is investigated combining laser ablation inductively coupled plasma mass spectrometry and the spatially resolved analysis of dried pL-droplets from a solution with a known concentration of Quantum Dots. Single cells and dried pL-droplets are morphologically characterized by Atomic Force Microscopy. A number concentration of CdSe/ZnS QDs between 3.5 104 and 48 104 is estimated to be uptaken by several selected single cells, after being incubated in the presence of a QDs suspension added to a standard cell culture medium. Mono-elemental bioimaging at subcellular resolution seems to show a higher number concentration of the CdSe/ZnS QDs in the cytosol around the cell nucleus.
KW - LA-ICP-SFMS
KW - Fast single pulse response
KW - Quantitative bioimaging
KW - Cellular uptake
KW - HT22
KW - HeLa
KW - Single cell
KW - pL-droplets
KW - CdSe/ZnS quantum Dots
KW - AFM
PY - 2021
DO - https://doi.org/10.1016/j.talanta.2021.122162
SN - 0039-9140
VL - 227
SP - 122162
PB - Elsevier B.V.
AN - OPUS4-52121
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Noureen, N.
A1 - Shah, F. A.
A1 - Lisec, Jan
A1 - Usman, H.
A1 - Khalid, M.
A1 - Munir, R.
A1 - Zaidi, N.
T1 - Revisiting the Association between Human Leukocyte Antigen and End-Stage Renal Disease
N2 - Multiple works have studied possible associations between human leukocyte antigen (HLA) alleles and end stage renal disease (ESRD). However, there are several contradictions in these previous works and no consistent HLA associations with ESRD itself have been identified. Most of these works have several limitations, for instance, the population size was too small, or only limited HLA loci were studied. The presented work aims to revisit the association between ESRD and HLA antigens while taking in to account the previously overlooked limitations. Here, we compared the HLA polymorphism (at HLA-A, -B, -C, -DRB1, -DQB1 and DQA1 loci) in ESRD patients (n=497) and controls (n=672). Our data identified several HLA alleles that displayed a significant positive or negative association with ESRD. We also determined whether heterozygosity or homozygosity of the ESRD-associated HLA alleles at different loci could modify the prevalence of the disease. Few HLA allele combinations displayed significant associations with ESRD among which HLA-A*3 –HLA-A*26 combination showed the highest strength of association (OR= 4.488, P≤ 0.05) with ESRD. However, the age of ESRD onset was not affected by HLA allele combinations at different loci. Most of the previous works have studied the association of HLA with ESRD in homogeneous ethnic groups and have interpreted their data accordingly. Here, we also performed an extensive literature analysis to determine whether the association of HLA to ESRD can be similar across different ethnic groups. This analysis showed that at least for certain alleles, the association of HLA to ESRD can be similar in different ethnic groups. For instance, HLA-A*11, HLA-DRB1*11, and HLA-DRB1*4 all showed significant positive associations with ESRD in different ethnic groups. The findings of our study will help in determining possible protective or susceptible roles of various HLA alleles in ESRD.
KW - Mass-Spectrometry
KW - HLA
KW - Renal disease
PY - 2020
DO - https://doi.org/10.1101/2020.03.18.996330
SP - 1
EP - 23
AN - OPUS4-50720
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rabin, Ira
ED - Binder, J.
T1 - The marginal notes of Tosefta MS Erfurt
N2 - Manuscript Erfurt 12 of the Tosefta (now Berlin, Staatsbibliothek, Ms. or. fol. 1220) is one of three major textual witnesses of the Tosefta. This manuscript has over 80 marginal notes which have not merited scholarly attention. This article presents a comprehensive analysis of all the marginal notes, including an evaluation of their ink composition, a palaeographic assessment of the scripts, as well as a philological assessment of their contents. Combining these methodologies differentiates between the glosses of the scribe and those added by later hands and identifies their provenance, allowing us to trace the history of the manuscript via the emendations that took place in the scholarly communities in which the manuscript was studied. One of the important outcomes of the research is an early dating of the manuscript to eleventh-century Italy, overturning the scholarly view which dates the manuscript to twelfth-century Rhineland
KW - Hebrew Manuscripts
KW - Ink
KW - NIR
KW - XRF
PY - 2025
DO - https://doi.org/10.3828/jjs.2025.76.2.272
SN - 0022-2097
VL - 76
IS - 2
SP - 272
EP - 300
AN - OPUS4-64770
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Homann, Christian
A1 - Peeters, Régis
A1 - Mirmajidi, Hana
A1 - Berg, Jessica
A1 - Fay, Michael
A1 - Rodrigues, Lucas Carvalho Veloso
A1 - Radicchi, Eros
A1 - Jain, Akhil
A1 - Speghini, Adolfo
A1 - Hemmer, Eva
T1 - Rapid microwave-assisted synthesis of morphology-controlled luminescent lanthanide-doped Gd2O2S nanostructures
N2 - Gadolinium oxysulfide (Gd2O2S) is an attractive material of demonstrated suitability for a variety of imaging applications, leveraging its magnetic, scintillating, and luminescent properties, particularly when doped with optically active lanthanide ions (Ln3+). For many of these applications, control over size and morphology at the nanoscale is crucial. This study demonstrates the rapid microwave-assisted Synthesis of colloidal Ln2O2S (Ln = Gd and dopants Yb, Er, Tb) nanostructures in as little as 20 min. Structural characterization using X-ray diffraction analysis (XRD), Raman spectroscopy, as well as Transmission electron microscopy (TEM), including elemental mapping via energy dispersive X-ray spectroscopy (EDS), unveiled the key role of elemental sulphur (S8) in the reaction mixtures for materials growth. By systematically varying the Ln-to-S ratio from 1 : 0.5 to 1 : 15, controlled morphologies ranging from triangular nanoplatelets to berry- and flower-like shapes were achieved. Doping with Er3+/Yb3+ endowed the nano-triangles with upconverting and near-infrared emitting properties. Tb3+-doped Gd2O2S exhibited the characteristic green Tb3+ emission under UV excitation, while also showing X-ray excited optical luminescence (XEOL), rendering the material interesting as a potential nano-scintillator.
KW - Upconversion
KW - Microwave-assisted synthesis
KW - Synthesis
KW - Fluorescence
KW - Nano
KW - Particle
KW - NIR
KW - XRD
KW - X-ray fluoressence
KW - Morphology control
KW - Raman
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647907
DO - https://doi.org/10.1039/D5TC01646K
SN - 2050-7526
VL - 13
IS - 35
SP - 18492
EP - 18507
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64790
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Putzu, Mara
A1 - Barbaresi, Marta
A1 - Fadda, Marta
A1 - Sacco, Alessio
A1 - Piergiovanni, Maurizio
A1 - Masino, Matteo
A1 - Bianchi, Federica
A1 - Altmann, Korinna
A1 - Benismail, Nizar
A1 - Coïc, Laureen
A1 - Fenoglio, Ivana
A1 - Mattarozzi, Monica
A1 - Rossi, Andrea Mario
A1 - Careri, Maria
A1 - Giovannozzi, Andrea Mario
T1 - Accuracy assessment of a micro-Raman spectroscopy method for small microplastic particles in infant milk formula
N2 - The presence of microplastics (MPs) in the food chain is increasingly documented, raising concerns over potential risks to human health. Despite growing efforts, standardized methods for MPs detection in food matrices remain limited. This study presents an interlaboratory comparison (ILC) aimed at assessing the accuracy and comparability of an analytical approach for the identification and quantification of small MPs (5–100 μm) in infant milk powder using μ-Raman spectroscopy and a representative polyethylene terephthalate (PET) reference material (RM). The RM, formulated as water-soluble tablets, was designed to replicate the morphology, size distribution, and polymer composition of environmentally relevant MPs, and was previously assessed for homogeneity and stability for mass fraction and particle numbers. The approach was assessed using two PET RM batches with different MPs particle numbers (high load batch: 1759 ± 141 MPs; low load batch: 160 ± 22 MPs), subjected to an enzymatic–chemical digestion, followed by μ-Raman analysis performed independently in two laboratories with different instruments and operators. Results are reported as absolute particle counts per analyzed sample and demonstrated excellent recovery across all size classes, including the smallest particles (down to 5 μm), with recovery rates ranging from 82 % to 88 %, in good agreement with the RM reference values. The analytical approach proved to be robust, reproducible, and suitable for low-level MPs quantification in complex food matrices, supporting ongoing efforts toward method harmonization and standardization for reliable MPs monitoring in the food sector.
KW - Microplastics
KW - Milk
KW - Raman microspectroscopy
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646239
DO - https://doi.org/10.1016/j.talo.2025.100586
SN - 2666-8319
VL - 12
SP - 1
EP - 8
PB - Elsevier B.V.
AN - OPUS4-64623
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Döring, Sarah
A1 - Tscheuschner, Georg
A1 - Flemig, Sabine
A1 - Weller, Michael G.
A1 - Konthur, Zoltán
T1 - Cost-Effective Method for Full-Length Sequencing of Monoclonal Antibodies from Hybridoma Cells
N2 - Background: Monoclonal antibodies play an important role in therapeutic and analytical applications. For recombinant expression, the coding sequences of the variable regions of the heavy and light chains are required. In addition, cloning antibody sequences, including constant regions, reduces the impact of hybridoma cell loss and ensures preservation of the naturally occurring full antibody sequence. Method: We combined amplification of IgG antibody variable regions from hybridoma mRNA with an advanced method for fulllength cloning of monoclonal antibodies in a simple two-step workflow. Following Sanger sequencing and evaluation of consensus sequences, the best matching variable, diversity,
and joining (V-(D-)J) gene segments were identified according to identity scores from IgBLAST reference sequences. Simultaneously, the mouse IgG subclass was determined at the DNA level based on isotype-specific sequence patterns in the CH1 domain. Knowing the DNA sequence of V-(D-)J recombination responsible for the complementary determining region 3 (CDR 3), variable region-specific primers were designed and used to amplify the corresponding antibody constant regions. Results: To verify the approach, we applied it to the hybridoma clone BAM-CCMV-29-81 and obtained identical full-length antibody
sequences as with RNA Illumina sequencing. Further validation at the protein level using an established MALDI-TOF MS-fingerprinting protocol showed that five out of six genetically encoded CDR domains of the monoclonal antibody BAM-CCMV-29-81 could be efficiently correlated. Conclusion: This simple, streamlined method enables the cost-effective determination of the full-length sequence of monoclonal antibodies from hybridoma cell lines, with the added benefit of obtaining the DNA sequence of the antibody ready for recombinant expression.
KW - Full-length antibody sequencing
KW - Hybridoma cell loss
KW - MALDI-TOF MS
KW - Immunoglobulin isotyping
KW - RNA Illumina sequencing
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639599
DO - https://doi.org/10.3390/antib14030072
SN - 2073-4468
VL - 14
IS - 3
SP - 1
EP - 17
PB - MDPI
CY - Basel
AN - OPUS4-63959
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ukrainczyk, Neven
A1 - Bernard, Thomas
A1 - Babaahmadi, Arezou
A1 - Huang, Liming
A1 - Zausinger, Christoph
A1 - Soive, Anthony
A1 - Bonnet, Stéphanie
A1 - Georget, Fabien
A1 - Mrak, Maruša
A1 - Dolenec, Sabina
A1 - Völker, Tobias
A1 - Suraneni, Prannoy
A1 - Wilson, William
T1 - Test methods for chloride diffusivity of blended cement pastes: a review by RILEM TC 298-EBD
N2 - The use of supplementary cementitious materials (SCM) is an important part of the roadmap for reducing CO2 emissions and extending the service life of reinforced concrete structures. To accelerate the adoption of SCMs, the RILEM Technical Committee 298-EBD evaluates scaled-down cement paste test methods to assess the effect of SCM on resistance to chloride and sulfate ingress and reactivity, which are critical to concrete durability. This review focuses on methods for measuring chloride diffusivity and is divided into four sections: diffusivity models and parameters, diffusion test methods (including NMR and chloride measurements), migration test methods and implications for future research. Key insights highlight the complexities of multi-species ionic and molecular diffusion/migration, including various binding interactions, and compares the different measurement methodologies. The review also addresses the test scale and aggregate effects, noting the pros and cons of testing at the paste, mortar, and concrete scales. The review underscores the need for further investigation into testing protocols and the influence of SCM on chloride diffusion, emphasizing that comprehensive testing across different scales provides complementary information for assessing durability performance.
KW - Chloride ingress
KW - Diffusion tests
KW - Migration test
KW - Cement paste
KW - Concrete
KW - Supplementary cementitious materials (SCM)
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645889
DO - https://doi.org/10.1617/s11527-025-02809-4
SN - 1359-5997
VL - 58
IS - 10
SP - 1
EP - 35
PB - Springer Science and Business Media LLC
AN - OPUS4-64588
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Desvergnes, Amélie Couvrat
A1 - Helman-Wazny, Agnieszka
T1 - Sialkoti paper used by Pahari artists: Raw materials and fibre analysis
N2 - This study aims to characterise the so-called Sialkoti paper used to produce Pahari drawings preserved today in the Wereldmuseum in Leiden (Netherlands) (WML). These works originate from the Punjab Hills in India (today Himachal Pradesh) and are commonly known as ‘Pahari miniature paintings’. The paper upon which these drawings are executed is said to have been produced in Sialkot during the eighteenth and nineteenth centuries when papermaking was an integral part of an overall regional economy correlated with other sectors such as agriculture and the textile industry. Although the term Sialkoti refers to identified papermills in Sialkot (now Pakistan), the paper from this region is yet to be subjected to a systematic study. This article therefore explores the paper(s) in question through macro- and microscopic observations of structure, pulp and fibres. The study of historical sources, complemented by the analysis of paper samples and fibre identification, has revealed that the pulp would have been prepared from a variety of manufactured products using different technologies, such as rags, cloth, mats, rope and other plant-based materials made from local bast fibres which, once tattered, were recycled to prepare the pulp. Microscopic study reveals that a variety of fibre combinations under different conditions and processing steps were used, in particular sunn hemp fibre (Crotalaria juncea L.), a plant species that has until now rarely been identified in historical paper. In addition, the presence of kenaf and jute fibres, as well as a significant quantity of cotton fibres, have also been demonstrated. To overcome the lack of comparative materials, our work was supported by a comparative study of several materials made from sunn hemp now held in the Ethnobotany Collection at Kew Gardens. Samples were taken from these materials and provided useful reference micrographs for the identification of the WML samples. The quality of the paper used by Pahari artists, as well as the raw materials available and their processing, are discussed in detail. Putting all the data, including technical and historical information into perspective, we conclude that the Pahari artists used a paper of inferior quality compared to other types of paper used for other purposes such as the creation of illuminated manuscripts in the Punjab plains. This study therefore provides useful analytical and material evidence that complements previous historical, technical and anthropological studies.
KW - Sialkoti paper
KW - Pahari drawings
KW - Indian handmade paper
KW - Sunn hemp
KW - Fibre identification
KW - Microscopy
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645216
DO - https://doi.org/10.1186/s40494-024-01360-9
SN - 2050-7445
VL - 12
SP - 1
EP - 18
PB - Springer
CY - Cham
AN - OPUS4-64521
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mirwald, Johannes
A1 - Khalighi, Sadaf
A1 - Varveri, Aikaterini
A1 - Hofko, Bernhard
A1 - Adwani, Dheeraj
A1 - Cannone-Falchetto, Augusto
A1 - Elwardany, Michael
A1 - Kleiziené, Rita
A1 - Konieczna, Katarzyna
A1 - Maliszewski, Maciej
A1 - Mouillet, Virginie
A1 - Nahar, Sayeda
A1 - Piérard, Nathalie
A1 - Pipintakos, Georgios
A1 - Porot, Laurent
A1 - Primerano, Kristina
A1 - Sharma, Aditi
A1 - Tavassoti, Pejoohan
A1 - Weigel, Sandra
A1 - Wetekam, Jens
A1 - Zhu, Jiqing
T1 - Evaluating the reproducibility and consistency of different sample preparation techniques used for ATR-FTIR spectroscopy from the RILEM 295-FBB TG1 round robin test
N2 - Attenuated Total Reflection Fourier Transform Infrared spectroscopy has become a popular spectroscopic technique in bituminous binder analysis. However, comparable results are not obtainable yet due to differences in devices, measurement routines, sample preparation procedures, and spectral evaluation. Thus, the Task Group 1 of the RILEM TC 295-FBB: “Fingerprinting bituminous binders using physicochemical analysis” focuses on bringing this method towards pre-standardization. This study evaluates the reproducibility and consistency from round robin test, where 21 participating laboratories performed six different preparation techniques on three different binders in an unaged, short-term, and long-term aged state. A total of 6461 spectra were recorded and evaluated for their mean, standard deviation and coefficient of variation (CV) in the spectral region between 1800 and 600 cm−1. The results show that the solid sample preparation methods provide excellent reproducibility, with a coefficient of variation below 2%. Only the solvent method showed a higher coefficient of variation at 7.18%. Outliers with a high CV were detected and categorized into two groups: one where only one of the four samples differed and the other where all 16 spectra showed slight scattering in the overall absorption. The consistency of the method is significantly influenced by the accuracy of sample preparation, which is crucial for minimizing differences in slope, baseline, and noise in the spectra. These findings show the excellent reproducibility of these sample preparation methods and will be further examined to establish universal indices for evaluating effects such as ageing, bringing the method closer towards standardization.
KW - Bitumen
KW - FTIR-Spektroskopie
KW - Reproducibility
KW - Round robin test
KW - Material handling
KW - preparation routine
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645386
DO - https://doi.org/10.1617/s11527-025-02755-1
SN - 1359-5997
VL - 58
IS - 8
SP - 1
EP - 21
PB - Springer Science and Business Media LLC
AN - OPUS4-64538
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Recknagel, Sebastian
A1 - Hoppe, Marion
A1 - Roik, Janina
T1 - Certification of a soda–lime–silica glass reference material for XRF-analysis
N2 - The preparation, analysis and certification of a new certified glass reference material (CRM) for multi-element determination in soda–lime–silica glass is described. The CRM BAM-S006 is available in the form of discs (thickness: 5 mm, diameter: 40 mm) as well as in form of cullet. Certified properties are the mass fractions of 19 main, minor and trace elements. The certified values are based on the results of 18 laboratories which participated in the certification inter-laboratory comparison. The CRM is intended for establishing or checking the calibration of x-ray spectrometers for the analysis of samples of similar matrix composition as well as for wet chemical analysis.
KW - reference material
KW - soda-lime-silica glass
KW - XRF-analysis
PY - 2025
DO - https://doi.org/10.13036/17533562.66.2.04
SN - 1753-3562
VL - 66
IS - 2
SP - 58
EP - 62
PB - Society of Glass Technology
CY - Sheffield, UK
AN - OPUS4-64543
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Altmann, Korinna
A1 - Portela, Raquel
A1 - Barbero, Francesco
A1 - Breuninger, Esther
A1 - Camassa, Laura Maria Azzurra
A1 - Velickovic, Tanja Cirkovic
A1 - Charitidis, Costas
A1 - Costa, Anna
A1 - Fadda, Marta
A1 - Fengler, Petra
A1 - Fenoglio, Ivana
A1 - Giovannozzi, Andrea M.
A1 - Haugen, Øyvind Pernell
A1 - Kainourgios, Panagiotis
A1 - von der Kammer, Frank
A1 - Kirchner, Markus J.
A1 - Lomax-Vogt, Madeleine
A1 - Lujic, Tamara
A1 - Milczewski, Frank
A1 - Moussawi, Mhamad Aly
A1 - Ortelli, Simona
A1 - Parac-Vogt, Tatjana N.
A1 - Potthoff, Annegret
A1 - Jimenez Reinosa, Julian J.
A1 - Röschter, Sophie
A1 - Sacco, Alessio
A1 - Wimmer, Lukas
A1 - Zanoni, Ilaria
A1 - Dailey, Lea Ann
T1 - Characterizing nanoplastic suspensions of increasing complexity: inter-laboratory comparison of size measurements using dynamic light scattering
N2 - Understanding the potential human health risks associated with micro- and nanoplastic exposure is currently a priority research area. Nanoplastic toxicity studies are complicated by the lack of available, well-characterized test and reference materials. Further, many nanoplastic test materials are inherently more polydisperse and heterogenous in shape compared to polystyrene beads, making accurate and representative size distribution measurements particularly challenging. The aim of this study was to conduct an inter-laboratory comparison of dynamic light scattering measurements, the most commonly used particle sizing method for nanomaterials. Using a published standard operating procedure, size measurements in water and a standardized cell culture medium (CCM) were generated for spherical, carboxy-functionalized polystyrene nanoparticles (PS-COOH; 50 nm; benchmark material), and for increasingly complex in-house produced spherical poly(ethylene terephthalate) (nanoPET) and irregular shaped polypropylene (nanoPP) test materials. The weighted mean of hydrodynamic diameters of PS-COOH dispersed in water (55 ± 5 nm) showed moderate variation between labs (coefficient of variation, CV = 8.2%) and were similar to literature reports. Measurements of nanoPET (82 ± 6 nm) and nanoPP (182 ± 12 nm) in water exhibited similar CV values (nanoPET: 7.3% and nanoPP; 6.8%). Dispersion of PS-COOH and nanoPET in CCM increased the CV to 15.1 and 14.2%, respectively, which is lower than literature reports (CV = 30%). We conclude with a series of practical recommendations for robust size measurements of nanoplastics in both water and complex media highlighting that strict adherence to a standard operating procedure is required to prevent particle agglomeration in CCM
KW - Nanoplastics
KW - Reference materials
KW - Polypropylene
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644571
DO - https://doi.org/10.1039/d5en00645g
SN - 2051-8153
SP - 1
EP - 15
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64457
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Billimoria, K.
A1 - Diaz Fernandez, Y. A.
A1 - Andresen, Elina
A1 - Sorzabal-Bellido, I.
A1 - Huelga-Suarez, G.
A1 - Bartczak, D.
A1 - Ortiz de Solórzano, C.
A1 - Resch-Genger, Ute
A1 - Goenaga Infante, H.
T1 - The potential of bioprinting for preparation of nanoparticle-based calibration standards for LA-ICP-ToF-MS quantitative imaging
N2 - This paper discusses the feasibility of a novel strategy based on the combination of bioprinting nano-doping technology and laser ablation-inductively coupled plasma time-of-flight mass spectrometry analysis for the preparation and characterization of gelatin- based multi-element calibration standards suitable for quantitative imaging. To achieve this, lanthanide up-conversion nanoparticles were added to a gelatin matrix to produce the bioprinted calibration standards. The features of this bioprinting approach were com- pared with manual cryosectioning standard preparation, in terms of throughput, between batch repeatability and elemental signal homogeneity at 5 μm spatial resolution. By using bioprinting, the between batch variability for three independent standards of the same concentration of 89 Y (range 0–600 mg/kg) was reduced to 5% compared to up to 27% for cryosectioning. On this basis, the relative standard deviation ( RSD ) obtained between three independent calibration slopes measured within 1 day also reduced from 16% (using cryosectioning ) to 5% (using bioprinting), supporting the use of a single standard preparation replicate for each of the concentrations to achieve good calibration performance using bioprinting. This helped reduce the analysis time by approximately 3-fold. With cryosectioning each standard was prepared and sectioned individually, whereas using bio-printing it was possible to have up to six different standards printed simultaneously, reducing the preparation time from approximately 2 h to under 20 min (by approxi- mately 6-fold). The bio-printed calibration standards were found stable for a period of 2 months when stored at ambient temperature and in the dark.
KW - Environmental analysis
KW - LA-ICP-MS
KW - Lanthanide
KW - Tag
KW - Fluorescence
KW - Nanoparticles
KW - Reference material
KW - Quality assurance
KW - 3D-printing
KW - Synthesis
KW - Production
KW - Multimodal
PY - 2022
DO - https://doi.org/10.1093/mtomcs/mfac088
SN - 1756-591X
VL - 14
IS - 12
SP - 1
EP - 9
PB - Oxford University Press
CY - Oxford
AN - OPUS4-57018
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sebald, M.
A1 - Gebauer, J.
A1 - Koch, Matthias
T1 - Concise Synthesis of Alternariol and Alternariol-9-monomethyl ether as well as their D3-Isotopologues
N2 - Abstract Alternariol (AOH) and alternariol-9-monomethyl ether (AME) are two secondary metabolites of Alternaria fungi which can be found in various foodstuff like tomatoes, nuts, and grains. Due to their toxicity and potential mutagenic activity the need for the development of high-throughput methods for the supervision of AOH- and AME-levels is of increasing interest. As the availability of both native and labeled AOH and AME analytical standards is very limited we herein wish to present a novel concise approach towards their synthesis employing a ruthenium-catalyzed ortho-arylation as the key step. Finally, we demonstrate their suitability as internal standards in stable-isotope dilution assay (SIDA)-HPLC-MS/MS analysis commonly used for the quantification of the natural products in food and feed.
KW - Mycotoxins
KW - Food Analysis
KW - Emerging contaminants
PY - 2021
DO - https://doi.org/10.1055/a-1698-8328
SN - 0039-7881
VL - 54
IS - 19
SP - 4285
EP - 4293
PB - Thieme
AN - OPUS4-53994
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Matiushkina, Anna
A1 - Abram, Sarah-Luise
A1 - Tavernaro, Isabella
A1 - Richstein, R.
A1 - Reithofer, M. R.
A1 - Andresen, Elina
A1 - Michaelis, Matthias
A1 - Koch, Matthias
A1 - Resch-Genger, Ute
T1 - Quantifying Citrate Surface Ligands on Iron Oxide Nanoparticles with TGA, CHN Analysis, NMR, and RP-HPLC with UV Detection
N2 - Although citrate is frequently used as a surface ligand for nanomaterials (NMs) such as metal, metal oxide, and lanthanide-based NMs in hydrophilic environments due to its biocompatibility and simple replacement by other more strongly binding ligands in postsynthetic surface modification reactions, its quantification on NM surfaces has rarely been addressed. Here, we present a multimethod approach for citrate quantification on iron oxide nanoparticles (IONPs) broadly applied in the life and material sciences. Methods explored include thermogravimetric (TGA) and elemental (CHN) analysis, providing citrate-nonspecific information on the IONP coating, simple photometry, and citrate-selective reversed-phase high-performance liquid chromatography (RP-HPLC) with absorption (UV) detection and quantitative nuclear magnetic resonance spectroscopy (qNMR). Challenges originating from the strongly absorbing magnetic NM and paramagnetic iron species interfering with optical and NMR Methods were overcome by suitable sample preparation workflows. Our multimethod approach to citrate quantification highlights the advantages of combining specific and unspecific methods for characterizing NM Surface chemistry and method cross-validation. It also demonstrates that chemically nonselective measurements can favor an overestimation of the amount of a specific surface ligand by signal contributions from molecules remaining on the NM surface, e.g., from particle synthesis, such as initially employed ligands and/or surfactants. Our results emphasize the potential of underexplored selective RPHPLC for quantifying ligands on NMs, which does not require a multistep sample preparation workflow such as qNMR for many NMs and provides a higher sensitivity. These findings can pave the road to future applications of versatile HPLC methods in NM characterization.
KW - Advanced material
KW - Functional group
KW - Iron oxide
KW - Ligand
KW - Nano
KW - Particle
KW - Quantification
KW - Surface analysis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648632
DO - https://doi.org/10.1021/acs.analchem.5c03024
SN - 0003-2700
VL - 97
IS - 36
SP - 19627
EP - 19634
PB - American Chemical Society (ACS)
CY - Washington, DC
AN - OPUS4-64863
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Billimoria, K.
A1 - Andresen, Elina
A1 - Resch-Genger, Ute
A1 - Goenaga-Infante, H.
T1 - A Strategy for Quantitative Imaging of Lanthanide Tags in A549 Cells Using the Ratio of Internal Standard Elements
N2 - One remaining handicap for spatially resolved elemental quantification in biological samples is the lack of a suitable internal standard (IS) that can be reliably measured across both calibration standards and samples. In this work, multielement quantitative intracellular imaging of cells tagged with lanthanide nanoparticles containing key lanthanides, e.g., Eu and Ho, is described using a novel strategy that uses the ratio of IS elements and LA-ICP-TOFMS analysis. To achieve this, an internal standard layer is deposited onto microscope slides containing either gelatin calibration standards or Euand Ho-tagged cell samples. This IS layer contains both gallium (Ga) and indium (In).
Monitoring either element as an IS individually showed significant variability in intensity signal between sample or standards prepared across multiple microscope slides, which is indicative of the difficulties in producing a homogeneous film at intracellular resolution.
However, normalization of the lanthanide signal to the ratio of the IS elements improved the calibration correlation coefficients from 0.9885 to 0.9971 and 0.9805 to 0.9980 for Eu and Ho, respectively, while providing a consistent signal to monitor the ablation behavior between standards and samples. By analyzing an independent quality control (QC) gelatin sample spiked with Eu and Ho, it was observed that without normalization to the IS ratio the concentrations of Eu and Ho were highly biased by approximately 20% in comparison to the expected values.
Similarly, this overestimation was also observed in the lanthanide concentration distribution of the cell samples in comparison with
the normalized data.
KW - Nanoparticle
KW - Nano
KW - Luminescence
KW - Quality assurance
KW - Synthesis
KW - Standardization
KW - Reference material
KW - ICP-MS
KW - LA-ICP-MS
KW - Quantification
KW - Bioimaging
PY - 2024
DO - https://doi.org/10.1021/acs.analchem.4c02763
SN - 0003-2700
VL - 96
IS - 30
SP - 12570
EP - 12576
AN - OPUS4-60768
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Jaeger, Carsten
A1 - Lintelmann, Jutta
A1 - Franke, Raimo
A1 - Artati, Anna
A1 - Cecil, Alexander
A1 - Broda, Frank
A1 - Klawonn, Frank
A1 - Erban, Alexander
A1 - Kopka, Joachim
A1 - Fuchs, Beate
A1 - Sommer, Ulf
A1 - Neumann-Schaal, Meina
A1 - O'Connor, Gavin
T1 - Analytical practices, use and needs of standard and reference materials in the German-speaking metabolomics community: results of an online survey
N2 - Introduction
Since the early 2000s, metabolomics has grown rapidly, becoming integral to fields like life sciences, health, and environmental research. This expansion has led to the formation of national and international societies, such as Germany’s DGMet, to tackle emerging challenges. One of DGMet’s goals is to improve measurement quality by assessing community needs for harmonization and standardization. A recent survey within the German-speaking community aimed to identify current practices and gaps in the use of chemical standards and reference materials, to guide future standardization efforts and collaborative initiatives.
Methods
An online survey was conducted between June 2023 and April 2024. The survey consisted of 38 key questions and was open to research institutions from Germany, Austria, and Switzerland.
Results
The survey was accessed by 68 laboratories, with 23 institutes providing complete or partial responses (34% response rate), which is comparable to rates reported in similar surveys within the metabolomics and lipidomics communities. Respondents were mainly experienced researchers from Germany, focusing mainly on health-related (“red”) metabolomics, as indicated by 78% of the respondents, followed by microbial (“grey”, 48%) and plant (“green”, 39%) metabolomics (multiple answers possible). The use of targeted methods was reported more frequently (91%) than that of non-targeted methods (78%), whereas metabolite fractions studied were equally split between polar, midpolar and lipid fractions (83% each). Human (74%), mouse (61%) and Arabidopsis (30%) were the most frequently studied organisms. Most participants used synthetic chemical standards for instrument qualification (83%), calibration (78%), and metabolite identification (74%), while matrix reference materials were mainly applied for quality control (52%) and method validation (44%). There was a strong demand for more standards, especially for metabolite identification and quantification, with cost being a major barrier, particularly for isotopically labelled standards and certified reference materials.
Conclusions
Valuable insights into the use of standards and reference materials within the German-speaking metabolomics community were obtained. Moving forward, the community should address critical gaps in metabolomics standardization. To achieve this, it must share its knowledge, articulate its needs clearly, and actively engage in joint efforts with national metrology institutes and international standardization initiatives.
KW - Reference material
KW - Chemical standard
KW - Metabolomics
KW - Mass spectrometry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647303
DO - https://doi.org/10.1007/s11306-025-02360-x
VL - 21
IS - 6
SP - 1
EP - 11
PB - Springer-Nature
CY - Heidelberg
AN - OPUS4-64730
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sebald, M.
A1 - Gebauer, J.
A1 - Koch, Matthias
T1 - Diastereoselective synthesis of (±)-trichodiene and (±)-trichodiene-D3 as analytical standards for the on-site quantification of trichothecenes
N2 - The ubiquitous Fusarium genus is responsible for the spoilage of vast amounts of cereals and fruits.
Besides the economic damage, the danger to human and animal health by the concomitant exposure to mycotoxins represents a serious problem. A large number of Fusarium species produce a variety of different mycotoxins of which the class of trichothecenes are of particular importance due to their toxicity.
Being identified as the common volatile precursor during the biosynthesis of trichothecenes, (−)-trichodiene (TD) is considered to be a biomarker for the respective mycotoxin content in food samples. We postulated that the development of a non-invasive, on-site GC-IMS method for the quantification of (−)-trichodiene supplemented with a stationary SIDA headspace GC-MS reference method would allow circumventing the laborious and expensive analyses of individual trichothecenes in large cereal samples.
In this work we present the syntheses of the required native calibration standard and an isotope labeled (TD-D3) internal standard.
KW - Mycotoxins
KW - Volatile marker
KW - Food analysis
KW - Screening method
KW - Mobile analysis
PY - 2021
DO - https://doi.org/10.1039/d1ob01778k
VL - 19
IS - 45
SP - 9872
EP - 9879
PB - RSC
AN - OPUS4-53993
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - You, Zengchao
A1 - Hoffmann, V.
A1 - Morcillo, Dalia
A1 - Agudo Jácome, Leonardo
A1 - Leonhardt, Robert
A1 - Winckelmann, Alexander
A1 - Richter, Silke
A1 - Recknagel, Sebastian
A1 - Abad Andrade, Carlos Enrique
T1 - Investigation of aluminum current collector degradation in lithium-ion batteries using glow discharge optical emission spectrometry
N2 - In this work, we employed glow discharge optical emission spectrometry (GD-OES) depth profiling as a fast and semi-quantitative method to investigate the aluminum (Al) current collector degradation in commercial lithium cobalt oxide (LCO) pouch cells with no Al2O3 pretreatment. After battery aging, a heterogeneous deposit was found on the surface of the cathode. Gray hotspot areas within an extensive pale white region were formed. Consistent with energy dispersive X-ray (EDX) analysis of micro-cross sections milled via targeted focused ion beam (FIB), an Al-containing layer of approximately 3 µm can be observed using GD-OES. We attribute one main cause of this layer is the degradation of the Al current collector. The nonuniform growth of this layer was investigated by performing GD-OES depth profiling at different in-plane positions. We found that the gray area has a higher mass concentration of Al, probably in metallic form, whereas the white area was probably covered more homogeneously with Al2O3, resulting from the inhomogeneous distribution of the pitting positions on the current collector. Compared to FIB-EDX, GD-OES enables a faster and more convenient depth profile analysis, which allows the more productive characterization of lithium-ion batteries (LIBs), and consequently benefits the development of preferable battery materials.
KW - GD-OES
KW - depth profiles
KW - Li-ion battery
KW - battery aging mechanism
KW - current collector corrosion
PY - 2023
DO - https://doi.org/10.1016/j.sab.2023.106681
SN - 0584-8547
VL - 205
SP - 106681
PB - Elsevier B.V.
CY - Amsterdam, Netherlands
AN - OPUS4-57383
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Duarte-Ruiz, D.
A1 - Saßnick, H.-D.
A1 - Ferreira De Araujo, F.
A1 - Gentzmann, Marie
A1 - Huthwelker, T.
A1 - Cocchi, C
T1 - X-ray absorption spectroscopy of scandium oxide polymorphs
N2 - Scandium oxide (Sc2O3) is a rare-earth oxide with significant potential in key technological areas, but due to its limited supply a deep understanding of its characteristics in different crystalline phases is still missing. Here, we present a combined experimental and ab initio X-ray absorption spectroscopy investigation of Sc2O3 focusing on excitations from the O K-edge and the Sc L2,3-edge. While measurements are performed on a cubic sample, the most stable phase under ambient conditions, six different polymorphs are computed, including two high-pressure phases with a trigonal and monoclinic lattice in addition to the cubic phase, as well as three computationally predicted structures. Our analysis of the structural and electronic properties reveals significant similarities between the cubic polymorph and the high-pressure trigonal phase, while the monoclinic crystal exhibits distinct features. The spectra simulated for these similar phases from the solution of the Bethe–Salpeter equation show very good agreement with measurements. Additional comparison with results computed in the independent-particle approximation highlights the dominant role of electron–hole correlations in shaping the absorption features, particularly at the O K-edge, where a common pattern with the features of other sesquioxides is identified. Our findings offer new insight into the spectral fingerprints of Sc2O3 polymorphs, aiding in situ characterization and informing sustainable materials management.
KW - Scandium
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650806
DO - https://doi.org/10.1039/d5ra06446e
VL - 15
IS - 56
SP - 47814
EP - 47825
AN - OPUS4-65080
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sun, Yijuan
A1 - Pérez-Padilla, Víctor
A1 - Valderrey, Virginia
A1 - Bell, Jérémy
A1 - Gawlitza, Kornelia
A1 - Rurack, Knut
T1 - Ratiometric detection of perfluoroalkyl carboxylic acids using dual fluorescent nanoparticles and a miniaturised microfluidic platform
N2 - The widespread contamination of soil and water with perfluoroalkyl substances (PFAS) has caused considerable societal and scientific concern. Legislative measures and an increased need for remediation require effective on-site analytical methods for PFAS management. Here we report on the development of a green-fluorescent guanidine-BODIPY indicator monomer incorporated into a molecularly imprinted polymer (MIP) for the selective detection of perfluorooctanoic acid (PFOA). Complexation of PFOA by the indicator, which is mediated by concerted protonation-induced ion pairing-assisted hydrogen bonding, significantly enhances fluorescence in polar organic solvents. The MIP forms as a thin layer on silica nanoparticles doped with tris(bipyridine)ruthenium(II) chloride, which provides an orange emission signal as internal reference, resulting in low measurement uncertainties. Using a liquid-liquid extraction protocol, this assay enables the direct detection of PFOA in environmental water samples and achieves a detection limit of 0.11 µM. Integration into an opto-microfluidic system enables a compact and user-friendly system for detecting PFOA in less than 15 minutes.
KW - PFAS
KW - Molecular imprinting
KW - Microfluidics
KW - Fluorescence
KW - Onsite assay
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650270
DO - https://doi.org/10.1038/s41467-025-66872-9
SN - 2041-1723
VL - 16
IS - 1
SP - 1
EP - 16
PB - Springer Science and Business Media LLC
AN - OPUS4-65027
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sathiyamani, S.
A1 - Ngiam, S.
A1 - Bonnerot, O.
A1 - Jaengsawang, S.
A1 - Panarut, P.
A1 - Helman-Wazny, Agnieszka
A1 - Colini, C.
T1 - Material Characterisation of 19–20th Century Manuscripts from Northern Thailand
N2 - Material analysis was carried out on four manuscripts from Northern Thailand, which included two palm-leaf manuscripts and two paper manuscripts. The two palm-leaf manuscripts MS 6 and MS 7 were found to have been written in the traditional method, wherein text was incised on the surface of the leaves, and then soot applied to the surfaces, confirmed by the identification of carbon ink. MS 7 additionally showed the presence of trace levels of iron in the ink, either from soot paste or from the stylus used for inscribing. The paper manuscript MS 3 was written in iron-gall ink, with sections written using a methyl-violet based ink while MS 4 was written in carbon ink. The paper used in the case of MS 3 was found to be machine made, while khoi fibres (Streblus asper) were used for making the paper used for MS 4. A combination of traditional and modern pigments, like molybdenum orange, was used for decorating the edges and cover. The results improved our understanding of these manuscripts in particular, and also provided us with insights about the rapid adoption of modern materials and their incorporation into the production of written artefacts from Northern Thailand in the late 19th and early 20th centuries.
KW - Materials analysis
KW - Paper manuscript
KW - Palm-leaf manuscript
KW - Writing inks
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652586
DO - https://doi.org/10.1515/res-2023-0028
SN - 0034-5806
VL - 45
IS - 2-3
SP - 117
EP - 140
PB - Walter de Gruyter GmbH
AN - OPUS4-65258
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Yusenko, Kirill
A1 - Stawski, Tomasz
A1 - Kulow, Anicó
A1 - Cakir, Cafer Tufan
A1 - Röder, Bettina
A1 - Naese, Christoph
A1 - Britzke, Ralf
A1 - Sintschuk, Michael
A1 - Emmerling, Franziska
T1 - BAMline - A real-life sample materials research beamline
N2 - With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research.
KW - Extended X-ray absorption fine structure
KW - Energy storage
KW - Environmental impacts
KW - Nondestructive testing techniques
KW - X-ray fluorescence spectroscopy
KW - Corrosion
KW - Near edge X-ray absorption fine structure spectroscopy
KW - X-ray absorption spectroscopy
PY - 2023
DO - https://doi.org/10.1063/5.0157194
VL - 158
IS - 24
SP - 1
EP - 22
PB - AIP Publishing
AN - OPUS4-57824
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - 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 - Lilensten, L.
A1 - Provost, K.
A1 - Perrière, L.
A1 - Fonda, E.
A1 - Couzinié, J.
A1 - Amman, F.
A1 - Radtke, Martin
A1 - Dirras, G.
A1 - Guillot, I.
T1 - Experimental investigation of the local environment and lattice distortion in refractory medium entropy alloys
N2 - EXAFS analysis of pure elements, binary and ternary equiatomic refractory alloys within the Nb-Zr-Ti-Hf- Ta system is performed at the Nb and Zr K-edges to analyze the evolution of the chemical local environ- ment and the lattice distortion. A good mixing of the elements is found at the atomic scale. For some compounds, a distribution of distances between the central atom and its neighbors suggests a distortion of the structure. Finally, analysis of the Debye-Waller parameters shows some correlation with the lat- tice distortion parameter δ², and allows to quantify experimentally the static disorder in medium entropy alloys.
KW - BAMline
KW - Refractory alloys
KW - EXAFS
KW - Debye-Waller parameter
PY - 2022
DO - https://doi.org/10.1016/j.scriptamat.2022.114532
SN - 1359-6462
VL - 211
SP - 1
EP - 6
PB - Elsevier Ltd.
AN - OPUS4-55287
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lutz, C.
A1 - Hampel, S.
A1 - Beuermann, S.
A1 - Turek, T.
A1 - Kunz, U.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Fittschen, U. E. A.
T1 - Investigation on Vanadium Species Distribution in Nafion™ 117 after Cyclization in a Vanadium Redox Flow Battery
N2 - The vanadium redox flow battery (VRFB) is currently a potential candidate for stationary energy storage. A major challenge is the unintended vanadium transport through the separator, which results in a fade of capacity. To overcome this issue, it is necessary to understand the transport processes in the membrane on a more fundamental level. In this work, the vanadium species distribution in Nafion™ 117 after cyclization was investigated. Two membranes, one from a charged VRFB and another from a discharged VRFB, were analyzed using ultraviolet–visible spectroscopy (UV/VIS) and X-ray absorption near edge structure spectroscopy (XANES). Little difference between the two membranes was recognizable according to the UV/VIS results. In comparison, the XANES results showed that the membrane from the charged VRFB contains more V3+ than VO2+, whereas for the discharged case, more VO2+ is present in the membrane.
KW - Synchrotron
KW - BAMline
KW - XANES
KW - Vanadium redox flow battery
PY - 2021
VL - 64
SP - 1
EP - 8
AN - OPUS4-54144
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Guerra, M.F.
A1 - Neri, E.
A1 - Radtke, Martin
T1 - Gold leaf tesserae: tracing the origins of gold using synchrotron-based techniques
N2 - To gain insight into the possible origin of the gold used in the production of tesserae containing gold leaf less than 0.5 μm thick placed between two layers of glass, we propose a non-destructive synchrotron radiation (SR) XRF protocol based on sequential analysis under optimised analytical conditions. Using this protocol, trace element analysis is achieved with detection limits of 1–6 mg/kg. As Pt and Au have adjacent fluorescence energies, we tested the most challenging situation, when Pt is present in very low concentrations in gold. Data obtained by double-dispersive XRF (D2XRF) and μXRF for fourth–ninth-century mosaics decorating nine Eastern and Western religious buildings show that the Eastern and Western tesserae are made from different alloys.
However, these alloys are identical to those used to make gold leaf for gilding, because plastic deformation requires the use of gold alloys with high ductility and malleability. Although trace element composition of gold used in the concerned period is only available for coins, by comparing the amounts of Pt contained in the tesserae and in the coins we show that Roman tesserae are made from Roman gold, as described in the documentary sources. We observe for the Byzantine period the use of a Byzantine gold and of gold supposedly from different stages of recycling, and we suggest the use of Umayyad and Abbasid gold for the production of Islamic tesserae.
KW - Gold
KW - XRF
KW - Synchrotron
KW - BAMline
KW - D2XRF
KW - Tesserae
PY - 2023
DO - https://doi.org/10.1140/epjp/s13360-022-03638-y
SN - 2190-5444
VL - 138
IS - 2
SP - 1
EP - 15
AN - OPUS4-57208
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Leidigkeit, Carolin
A1 - Shokr, Mohammad
A1 - Tosson, Amir
A1 - Cakir, Cafer Tufan
A1 - Radtke, Martin
A1 - Pietsch, Ullrich
A1 - Christ, Hans-Jürgen
T1 - Using Energy-Dispersive Laue Diffraction to Study Dislocation Arrangements in Materials Showing Wavy and Planar Slip Behavior
N2 - The present work shows an approach to monitor the evolution of the dislocation arrangement of a metallic material caused by cyclic plastic strain using white X-ray radiation in combination with an energy-dispersive detector. The method is demonstrated by single-shot experiments performed on polycrystalline nickel and α-brass, representing the pure wavy and the pure planar dislocation slip behavior. To correlate the resulting diffraction patterns with various dislocation arrangements of both metals, fatigue tests were carried out up to certain numbers of cycles and at predetermined plastic strain amplitudes. The differences in dislocation microstructure and internal stress distributions give rise to an appreciable change in the peak shape of Laue reflections, leading to unique characteristics in the respective diffraction patterns. Nickel reflections are elongated due to the high amount of cell structures leading to bending and misorientation of the lattice, whereas the present stacking faults in α-brass result in powder-like diffraction.
KW - Slip behavior
KW - Energy-Dispersive
KW - Laue Diffraction
KW - Dislocation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637964
DO - https://doi.org/10.1111/ffe.14535
SN - 1460-2695
VL - 48
IS - 3
SP - 1341
EP - 1351
PB - Wiley
AN - OPUS4-63796
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 - JOUR
A1 - Grzelec, Małgorzata
A1 - Haas, Sylvio
A1 - Helman-Ważny, Agnieszka
T1 - Application of scanning small-angle X-ray scattering in the identification of sheet formation techniques in historical papers
N2 - Among writing substrates produced historically in different regions of the world, paper is one of the most complex materials. Its complexity results not only from a variety of highly processed ingredients, which can be used in its production, but also from a variety of methods in which these materials are combined to form the fibrillar network referred to as paper. While material identification methods are well established in the analysis of historical papers, the identification of manufacturing technologies is still an under-researched topic, that requires the development of appropriate methods and measurement protocols. This paper reports on the results of a research project aimed at the application of synchrotron scanning small angle X-ray scattering (SAXS) method in the characterization of paper structure, with emphasis on the assessment of fibrillar orientation as a marker characteristic for different, historical papermaking technologies. The main objective of this study consists of the development of a measurement protocol involving the SAXS technique complemented by other analytical methods in the characterization of the fibrous paper structure.
KW - SAXS
KW - Paper analysis
KW - Papermaking technology
KW - Fiber orientation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651594
DO - https://doi.org/10.1007/s00339-024-08157-4
SN - 0947-8396
VL - 131
IS - 1
SP - 1
EP - 16
PB - Springer Science and Business Media LLC
AN - OPUS4-65159
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Westwood, S.
A1 - Josephs, R. D.
A1 - Choteau, T.
A1 - Martos, G.
A1 - Wielgosz, R.
A1 - Sarzuri, Y. A.
A1 - Mendoza, E.
A1 - do Rego, E. C. P.
A1 - Violante, F. G. M.
A1 - da Silva Souza, W.
A1 - de Carvalho, L. J.
A1 - Fernandes, J. L. N.
A1 - Bates, J.
A1 - Rajotte, I.
A1 - Melanson, J. E.
A1 - Li, H.
A1 - Guo, Z.
A1 - Su, F.
A1 - Wang, S.
A1 - Huang, T.
A1 - Lalerle, B.
A1 - Gantois, F.
A1 - Piechotta, Christian
A1 - Philipp, Rosemarie
A1 - Kaminski, Katja
A1 - Klyk-Seitz, Urzsula-Anna
A1 - Giannikopoulou, P.
A1 - Skotidaki, E.
A1 - Kakoulides, E.
A1 - Pui-Kwan, C.
A1 - Kuroe, M.
A1 - Itoh, N.
A1 - Calderón, M. A. A.
A1 - Contreras, L. R.
A1 - Osuna, M. A.
A1 - Alrashed, M.
A1 - Ting, L.
A1 - Mei, G. E.
A1 - Juan, W.
A1 - Sze, C. P.
A1 - Lin, T. T.
A1 - Quinn, L.
A1 - Swiegelaar, C.
A1 - Fernandes-Whaley, M.
A1 - Ahn, S.
A1 - Chaiphet, T.
A1 - Sudsiri, N.
A1 - Bellazreg, W.
A1 - Bilsel, M.
A1 - Colombo, G.
T1 - Key comparison CCQM-K78.b - non-polar analytes in organic solvent: methoxychlor and trifluralin in acetonitrile
N2 - The CCQM-K78.b key comparison was coordinated by the Bureau International des Poids et Mesures (BIPM) on behalf of the CCQM Organic Analysis Working Group (OAWG) of the 'Comité Consultatif pour la Quantité de Matière' (CCQM), for National Measurement Institutes (NMIs) and Designated Institutes (DIs) providing measurement services in organic analysis under the 'Comité International des Poids et Mesures' (CIPM) Mutual Recognition Arrangement (MRA).
This key comparison was conducted as a 'Track A' comparison within the OAWG's 10-year strategic plan. The goal of CCQM-K78.b was to underpin capabilities for the value assignment of calibration solutions containing low polarity/non-polar organic analytes in organic solvents. The selected model system consisted of a two-component pesticide solution in acetonitrile, comprising methoxychlor and trifluralin.
Participants were tasked with assigning the mass fractions, in units of μg/g, of methoxychlor and trifluralin in acetonitrile solution. The mass fraction levels and analytical challenges of the selected analytes were representative of those encountered for calibration solutions of non-polar organic analytes. Participation in CCQM-K78.b allowed for the benchmarking of capabilities for assigning the mass fraction of non-polar organic compounds (pKow < -2) in solution, at mass fractions above 5 μg/g, in an organic solvent. Additionally, the comparison assessed the capabilities for the quantitative assignment of thermally labile compounds.
Participants were provided by the BIPM with ampoules containing methoxychlor and trifluralin in acetonitrile. Each participant reported the mass fraction content of each analyte in μg/g. All participants ensured the metrological traceability of their results through the use of a Primary Reference Material (PRM), which was used to prepare a primary calibrator solution for each analyte using a gravimetric procedure. The twenty participating institutes primarily used analysis procedures based on GC-MS, -IDMS, -MS/MS, -ECD, and -FID, with some participants also using LC-UV for the value assignment.
The analysis of methoxychlor and trifluralin in acetonitrile solution presented several challenges, including the thermal stability of the analytes under selected analytical techniques, control of solvent volatility, and considerable variation in some results using MS-based quantification methods. The mass fraction assignments for methoxychlor and trifluralin, consistent with the key comparison reference values (KCRVs), were achieved with associated relative standard uncertainties of (0.38 - 2.9) % for methoxychlor and (0.35 - 2.5) % for trifluralin.
To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.
The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
KW - Methoxychlor
KW - Trifluralin
KW - CCQM
KW - Key comparison
PY - 2025
DO - https://doi.org/10.1088/0026-1394/62/1A/08010
SN - 0026-1394
VL - 62
IS - 1A
SP - 1
EP - 37
PB - IOP Publishing
AN - OPUS4-64691
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rua-Ibarz, Ana
A1 - Nakadi, Flávio V.
A1 - Bolea-Fernandez, Eduardo
A1 - Bazo, Antonio
A1 - Battistella, Beatrice
A1 - Matiushkina, Anna
A1 - Resch-Genger, Ute
A1 - Abad Andrade, Carlos Enrique
A1 - Resano, Martín
T1 - Discrete entity analysis via microwave-induced nitrogen plasma–mass spectrometry in single-event mode
N2 - In this work, single-event microwave-induced nitrogen plasma–mass spectrometry (single-event MINP-MS) was evaluated for the first time for the analysis of discrete entities such as nanoparticles, biological cells, and microplastics. Nitrogen (N2) effectively overcomes Ar-based polyatomic interferences, enabling (ultra)trace element determination of Fe and Se using their most abundant isotopes, 56Fe (91.66%) and 80Se (49.82%). Iron oxide nanoparticles (Fe2O3 NPs) ranging from 20 to 70 nm were accurately characterized, with excellent agreement with established sizing techniques, such as transmission electron microscopy (TEM) and dynamic light scattering (DLS). A limit of detection (LoD) of 8.6 ag for Fe─equivalent to an LoDsize of 19 nm for Fe2O3─was achieved, which is significantly lower than recent values reported for high-end quadrupole-based ICP-MS. Selenium nanoparticles (SeNPs) of 150 and 250 nm were also accurately characterized, without the N2-based plasma experiencing issues handling relatively large metallic NPs (linearity, R2 = 0.9994). Se-enriched yeast cells (SELM-1 certified reference material) were successfully analyzed via single-cell MINP-MS using external calibration based on SeNPs and a transport efficiency-independent approach. In addition, 2–3 μm polystyrene (PS) and polytetrafluoroethylene (PTFE) were accurately sized by monitoring 12C+, confirming the method’s suitability for handling micrometer-sized polymeric materials (microplastics). The average duration of individual events (680 ± 160 μs) suggests that the digestion of individual entities in N2-based plasmas is comparable to that in Ar-based plasmas. These results open new avenues for this instrumentation as an alternative to ICP ionization sources, also in the context of discrete entity analysis.
KW - Microwave-Induced Nitrogen Plasma
KW - Discrete entity analysis
KW - Particle/droplet event counting
KW - Comparison to SP-ICP-MS methodologies
KW - Nitrogen plasma vs. argon ICP trade-offs
KW - Trace elemental quantification at the single-entity level
KW - Time-resolved mass spectrometry for discrete entities
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643825
DO - https://doi.org/10.1021/acs.analchem.5c04341
SN - 0003-2700
SP - 1
EP - 8
PB - American Chemical Society (ACS)
AN - OPUS4-64382
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Morcillo, Dalia
A1 - Winckelmann, Alexander
A1 - Oelze, Marcus
A1 - Leonhardt, Robert
A1 - Schmidt, Anita
A1 - Richter, Silke
A1 - Recknagel, Sebastian
A1 - Vogl, Jochen
A1 - Panne, Ulrich
A1 - Abad Andrade, Carlos Enrique
T1 - Exploring Age-Induced Lithium Isotope Fractionation in Lithium-Ion Batteries using Microwave-Induced Cold Nitrogen Plasma Mass Spectrometry
N2 - This study explores Microwave-Inductively Coupled Atmospheric-pressure Plasma Mass Spectrometry (MICAP-MS) as a cost-effective alternative to Multi-Collector Inductively Coupled Plasma Mass Spectrometry (MC-ICP-MS) for analyzing lithium isotopic composition in lithium-ion batteries (LIBs). We investigate the performance of MICAP-MS in measuring Li isotope ratios in new and aged commercial lithium cobalt oxide (LCO) batteries. Our results show that MICAP-MS, operating under cold plasma conditions at 800 W with an 8 mm torch position, achieves results metrologically compatible with MC-ICP-MS, with a precision ranging from 0.6‰ to 3.4‰ for δ7Li values. MICAP-MS benefits from a dielectric resonator for uniform plasma, better ion velocity control, and higher energy efficiency. Optimal settings were identified with dwell times of 10 ms for 6Li and 1 ms for 7Li. The study of LIBs revealed that 6Li migrates towards the anode over multiple charge–discharge cycles, causing 7Li to accumulate in the cathode, a fractionation effect that becomes more pronounced with prolonged cycling. MICAP-MS provides a cost-effective, precise alternative to MC-ICP-MS, with lower operational costs and enhanced portability, advancing the study of isotopic fractionation and aging in lithium-ion batteries.
KW - MICAP-MS
KW - Lithium
KW - Battery aging
KW - Lithium isotopes
KW - Nitrogen plasma
KW - Isotope fractionation
KW - lithium cobalt oxide
KW - LCO
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643777
DO - https://doi.org/10.1039/d4ja00324a
SN - 0267-9477
SP - 1
EP - 11
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64377
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Abad Andrade, Carlos Enrique
A1 - Jegielka, Dennis
A1 - Aloysius, Allen
A1 - Recknagel, Sebastian
T1 - SI-traceable total analysis of nitrate and nitrite by isotope dilution optical spectroscopy and its application to Berlin surface waters
N2 - Accurate nitrate and nitrite data support water-quality regulation, yet routine methods rely on external calibration and rarely achieve SI traceability. We report a calibration-free determination of nitrate and nitrite by combining isotope dilution with high-resolution continuum-source graphite furnace molecular absorption spectrometry (ID-HR-CS-GF-MAS). A 15N-enriched nitrate spike (its concentration verified by reverse isotope dilution against the standard reference material NIST 3185) provides the SI link, and it is gravimetrically added to samples; nitrate and residual nitrite are converted in situ to nitric oxide (NO), whose 215 nm band is recorded at a pixel resolution of λ/Δλ ≈ 140 000. The 0.2127 nm shift between 14NO and 15NO electronic spectra is resolved, and a three-latent-variable partial least squares regression model yields the 15N/14N ratio with 0.3% precision. Instrumental LoD values of 4.8 ng (14N) and 3.2 ng (15N) translate to a method LoD of 4.8 ng of nitrogen (equivalent to 1.05 mg L−1 NO3− for a 20 μL aliquot). The furnace program allows for successive drying/pyrolysis loops, so additional 20 μL aliquots can be layered onto the graphite platform. Alternatively, a 10 mL anion-exchange solid-phase extraction step concentrates nitrate and nitrite fivefold, allowing for the analysis of even lower sample concentrations. Results for four certified reference materials (2.9 to 1000 mg L−1 NO3−) agreed with certified values, giving relative expanded uncertainties of 2 to 4%. Analysis of twenty Berlin surface-water samples revealed concentrations ranging from 0.10 to 7.3 mg L−1 NO3−, indicating that the Panke River and Teltow Canal are the primary sources of nitrogen. ID-HR-CS-GF-MAS thus delivers ID-MS-level accuracy in a few minutes per run with bench-top optics, and, with optional on-platform or SPE pre-concentration, extends SI-traceable nitrate/nitrite monitoring into the low-ng regime.
KW - Isotope dilution
KW - Nitrate and nitrite determination
KW - SI-traceable quantification
KW - Calibration-free analysis
KW - Water quality
KW - Berlin surface waters
KW - NO molecular absorption bands
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643785
DO - https://doi.org/10.1039/D5JA00252D
SN - 0267-9477
VL - 40
IS - 10
SP - 2692
EP - 2701
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64378
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tavernaro, Isabella
A1 - Rajotte, Isabelle
A1 - Thibeault, Marie-Pier
A1 - Sander, Philipp C.
A1 - Kodra, Oltion
A1 - Lopinski, Gregory
A1 - Radnik, Jörg
A1 - Johnston, Linda J.
A1 - Brinkmann, Andreas
A1 - Resch-Genger, Ute
T1 - Quantifying surface groups on aminated silica nanoparticles of different size, surface chemistry, and porosity with solution NMR, XPS, optical assays, and potentiometric titration
N2 - We assessed the quantification of surface amino functional groups (FGs) for a large set of commercial and custom-made aminated silica nanoparticles (SiO2 NPs) with sizes of 20–100 nm, prepared with different sol–gel routes, different amounts of surface amino FGs, and different porosity with four methods providing different, yet connected measurands in a bilateral study of two laboratories, BAM and NRC, with the overall aim to develop standardizable measurements for surface FG quantification. Special emphasis was dedicated to traceable quantitative magnetic resonance spectroscopy (qNMR) performed with dissolved SiO2 NPs. For the cost efficient and automatable screening of the amount of surface amino FGs done in a first step of this study, the optical fluorescamine assay and a potentiometric titration method were utilized by one partner, i.e., BAM, yielding the amount of primary amino FGs accessible for the reaction with a dye precursor and the total amount of (de)protonatable FGs. These measurements, which give estimates of the minimum and maximum number of surface amino FGs, laid the basis for quantifying the amount of amino silane molecules with chemo-selective qNMR with stepwise fine-tuned workflows, involving centrifugation, drying, weighting, dissolution, measurement, and data evaluation steps jointly performed by BAM and NRC. Data comparability and relative standard deviations (RSDs) obtained by both labs were used as quality measures for method optimization and as prerequisites to identify method-inherent limitations to be later considered for standardized measurement protocols. Additionally, the nitrogen (N) to silicon (Si) ratio in the near-surface region of the SiO2 NPs was determined by both labs using X-ray photoelectron spectroscopy (XPS), a well established surface sensitive analytical method increasingly utilized for microparticles and nano-objects which is currently also in the focus of international standardization activities. Overall, our results underline the importance of multi-method characterization studies for quantifying FGs on NMs involving at least two expert laboratories for effectively identifying sources of uncertainty, validating analytical methods, and deriving NM structure–property relationships.
KW - Advanced Materials
KW - Amino Groups
KW - Calibration
KW - Characterization
KW - Functional groups
KW - Method Comparison
KW - Nano Particle
KW - Validation
KW - XPS
KW - Optical Assay
KW - Quantification
KW - Surface Analysis
KW - Reference Materials
KW - Synthesis
KW - Fluorescence
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649992
DO - https://doi.org/10.1039/d5na00794a
VL - 7
IS - 21
SP - 6888
EP - 6900
PB - Royal Society of Chemistry
AN - OPUS4-64999
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - 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 - Margreiter, R.
A1 - Baumann, J.
A1 - Mantouvalou, I.
A1 - Radtke, Martin
A1 - Reinholz, Uwe
A1 - Strub, E.
T1 - Investigations on fire-gilding
N2 - Fire-gilding is a historic technique for the application of golden layers on a number of different base materials utilizing a gold amalgam. This technique leaves a significant amount of Hg in the golden layer, giving archeometrists a reliable indicator to identify firegildings.
Recent findings on presumably fire-gilded objects have shown in several cases significantly lower Hg content than previously studied objects. This prompted a synchrotron-based X-ray fluorescence investigation into the Hg distribution along the material–gilding interface, as well as a series of measurements regarding the Hg content development in fire-gilded samples during artificial aging. This work presents findings on laboratory-prepared fire-gildings, indicating an Hg enrichment at the interface of firegilded silver samples. Notably, such an enrichment is missing in fire-gilded copper samples. Further, it is confirmed that fire-gilded layers typically do not undercut an Hg bulk content of 5%. In this light, it seems improbable that ancient samples that contain <5% Hg are fire-gilded. The results presented in this study might lead to a non-destructive method to identify the Hg enrichment at the interface. This might be obtained by a combination of different non-destructive measurements and might also work unambiguously in samples in which the gold top layer is altered.
KW - BAMline
KW - X-Ray Fluorescence
KW - Gilding
KW - Depth profile
KW - Archaeometry
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552885
DO - https://doi.org/10.1111/arcm.12797
SN - 0003-813X
SP - 1
EP - 14
PB - Wiley online library
AN - OPUS4-55288
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dobosy, Péter
A1 - Nguyen, Hoang Thi Phuong
A1 - Záray, Gyula
A1 - Streli, Christina
A1 - Ingerle, Dieter
A1 - Ziegler, Philipp
A1 - Radtke, Martin
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Endrédi, Anett
A1 - Fodor, Ferenc
T1 - Effect of iodine species on biofortification of iodine in cabbage plants cultivated in hydroponic cultures
N2 - Iodine is an essential trace element in the human diet because it is involved in the synthesis of thyroid hormones. Iodine deficiency affects over 2.2 billion people worldwide, making it a significant challenge to find plant-based sources of iodine that meet the recommended daily intake of this trace element. In this study, cabbage plants were cultivated in a hydroponic system containing iodine at concentrations ranging from 0.01 to 1.0 mg/L in the form of potassium iodide or potassium iodate. During the experiments, plant physiological parameters, biomass production, and concentration changes of iodine and selected microelements in different plant parts were investigated. In addition, the oxidation state of the accumulated iodine in root samples was determined. Results showed that iodine addition had no effect on photosynthetic efficiency and chlorophyll content. Iodide treatment did not considerably stimulate biomass production but iodate treatment increased it at concentrations less than 0.5 mg/L. Increasing iodine concentrations in the nutrient solutions increased iodine content in all plant parts; however, the iodide treatment was 2–7 times more efficient than the iodate treatment. It was concluded, that iodide addition was more favourable on the target element accumulation, however, it should be highlighted that application of this chemical form in nutrient solution decreased the concetrations of selected micoelement concentration comparing with the control plants. It was established that iodate was reduced to iodide during its uptake in cabbage roots, which means that independently from the oxidation number of iodine (+ 5, − 1) applied in the nutrient solutions, the reduced form of target element was transported to the aerial and edible tissues.
KW - BAMline
KW - XANES
KW - Synchrotron
KW - Lodine
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608330
DO - https://doi.org/10.1038/s41598-024-66575-z
VL - 14
IS - 1
SP - 1
EP - 12
PB - Springer Science and Business Media LLC
AN - OPUS4-60833
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Huang, Junhao
A1 - Klahn, Marcus
A1 - Tian, Xinxin
A1 - Bartling, Stephan
A1 - Zimina, Anna
A1 - Radtke, Martin
A1 - Rockstroh, Nils
A1 - Naliwajko, Pawel
A1 - Steinfeldt, Norbert
A1 - Peppel, Tim
A1 - Grunwaldt, Jan‐Dierk
A1 - Logsdail, Andrew J.
A1 - Jiao, Haijun
A1 - Strunk, Jennifer
T1 - Fundamental Structural and Electronic Understanding of Palladium Catalysts on Nitride and Oxide Supports
N2 - The nature of the support can fundamentally affect the function of a heterogeneous catalyst. For the novel type of isolated metal atom catalysts, sometimes referred to as single‐atom catalysts, systematic correlations are still rare. Here, we report a general finding that Pd on nitride supports (non‐metal and metal nitride) features a higher oxidation state compared to that on oxide supports (non‐metal and metal oxide). Through thorough oxidation state investigations by X‐ray absorption spectroscopy (XAS), X‐ray photoelectron spectroscopy (XPS), CO‐DRIFTS, and density functional theory (DFT) coupled with Bader charge analysis, it is found that Pd atoms prefer to interact with surface hydroxyl group to form a Pd(OH)x species on oxide supports, while on nitride supports, Pd atoms incorporate into the surface structure in the form of Pd−N bonds. Moreover, a correlation was built between the formal oxidation state and computational Bader charge, based on the periodic trend in electronegativity.
KW - BAmline
KW - XANES
KW - Catalyst
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608341
DO - https://doi.org/10.1002/anie.202400174
SN - 1433-7851
VL - 63
IS - 20
SP - 1
EP - 9
PB - Wiley
AN - OPUS4-60834
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Senges, Gene
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Lindič, Tilen
A1 - Gully, Tyler A.
A1 - Winter, Marlon
A1 - Radtke, Martin
A1 - Röder, Bettina
A1 - Steinhauer, Simon
A1 - Paulus, Beate
A1 - Emmerling, Franziska
A1 - Riedel, Sebastian
T1 - Unravelling highly oxidized nickel centers in the anodic black film formed during the Simons process by in situ X-ray absorption near edge structure spectroscopy
N2 - The electrofluorination after Simons has been used for the last century to produce everyday life materials. An in situ XANES investigation of the controversially debated black film apparent in the Simons process revealed high-valent nickel centers.
KW - Synchrotron
KW - BAMline
KW - XANES
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608366
DO - https://doi.org/10.1039/d3sc06081k
SN - 2041-6520
VL - 15
IS - 12
SP - 4504
EP - 4509
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-60836
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 - JOUR
A1 - Moufid, M.
A1 - Bouchikhi, B.
A1 - Tiebe, Carlo
A1 - Bartholmai, Matthias
A1 - El Bari, N.
T1 - Assessment of outdoor odor emissions from polluted sites using simultaneous thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS), electronic nose in conjunction with advanced multivariate statistical approaches
N2 - Poor air quality, particularly in urban areas, causes various diseases and degrades living standards. Air Quality could be affected by emissions of odor, Volatile Organic Compounds (VOCs), and other gases. Therefore, assessment and monitoring of odorous air quality using sensitive, simple, rapid, accurate and portable tools is very important for public health. This study aimed to characterize odor emissions to detect malfunctions in facilities and to prevent air pollution and olfactory nuisance in the environment. A gas chromatographic method, in conjunction with sensorial analysis were performed for odorous air samples analysis collected from neighborhood of Meknes city (Morocco). Advanced multivariate statistical approaches, such as Principal Components Analysis (PCA), Discriminant Function Analysis (DFA), Support Vector Machines (SVMs), and Hierarchical Cluster Analysis (HCA), were used to describe samples similarities. The electronic nose (e-nose) data processing exhibits a satisfactory discrimination between the odorous air samples. Twenty-four VOCs with known molecular formulas were identified with Thermal Desorption-Gas Chromatography-Mass Spectrometry (TD-GC-MS). A validated Partial Least Square (PLS) model foresees good calibration between e-nose measurement and TD-GCMS analysis. The finding indicates that TD-GC–MS approach in conjunction with e-nose unit could be suitable tool for environmental measurement-based odor emissions.
KW - Electronic nose
KW - TD-GC-MS
KW - PLS regression
KW - Multivariate analysis
KW - Outdoor odor emissions
PY - 2021
DO - https://doi.org/10.1016/j.atmosenv.2021.118449
SN - 1352-2310
VL - 256
SP - 118449
PB - Elsevier Ltd.
AN - OPUS4-52626
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kazlagić, Anera
A1 - Vogl, Jochen
A1 - Gluth, Gregor
A1 - Stephan, D.
T1 - Provenancing of cement using elemental analyses and isotope techniques – The state-of-the-art and future perspectives
N2 - With the aim of identifying the origin and the manufacturer of a cement, a reliable procedure that provides unambiguous results is needed. Such procedure could resolve practical issues in damage research, liability issues and forensic investigations. A substantial number of attempts for fingerprinting of building materials, including cement, has already been carried out during the last decades. Most of them were based on concentration analysis of the main elements/components. This review provides an overview of provenance studies of cement and the main approaches commonly used. Provenance studies of cement via isotope techniques are also presented and discussed as representatives of the state-of-the-art in the field. Due to the characteristic properties and the occurrence of carefully selected isotope ratios, unique fingerprints of different kinds of materials can be provided by these methods. This property has largely been explored in various scientific fields such as geo- and cosmochemistry, food forensics, archaeology, geochronology, biomedical studies, and climate change processes. However, the potential of isotope techniques in cement and concrete research for provenance studies has barely been investigated.
Therefore, the review outlines a suitable approach using isotope ratios, which could lead to reliable provenancing of cementitious materials in the future.
KW - Cement
KW - Sr isotopes
KW - Provenance
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533762
DO - https://doi.org/10.1039/d1ja00144b
VL - 36
IS - 10
SP - 2030
EP - 2042
PB - The Royal Society of Chemistry
CY - Cambridge, UK
AN - OPUS4-53376
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 - JOUR
A1 - Kazlagić, Anera
A1 - Russo, Francesco
A1 - Vogl, Jochen
A1 - Sturm, Patrick
A1 - Stephan, D.
A1 - Gluth, Gregor
ED - Resch-Genger, Ute
ED - Koch, Matthias
ED - Meermann, Björn
ED - Weller, Michael G.
T1 - Development of a sample preparation procedure for Sr isotope analysis of Portland cements
N2 - The 87Sr/86Sr isotope ratio can, in principle, be used for provenancing of cement. However, while commercial cements consist of multiple components, no detailed investigation into their individual 87Sr/86Sr isotope ratios or their influence on the integral 87Sr/86Sr isotope ratio of the resulting cement was conducted previously. Therefore, the present study aimed at determining and comparing the conventional 87Sr/86Sr isotope ratios of a diverse set of Portland cements and their corresponding Portland clinkers, the major component of these cements. Two approaches to remove the additives from the cements, i.e. to measure the conventional 87Sr/86Sr isotopic fingerprint of the clinker only, were tested, namely, treatment with a potassium hydroxide/sucrose solution and sieving on a 11-µm sieve. Dissolution in concentrated hydrochloric acid/nitric acid and in diluted nitric acid was employed to determine the 87Sr/86Sr isotope ratios of the cements and the individual clinkers. The aim was to find the most appropriate sample preparation procedure for cement provenancing, and the selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated cements with those of the corresponding clinkers. None of the methods to separate the clinkers from the cements proved to be satisfactory. However, it was found that the 87Sr/86Sr isotope ratios of clinker and cement generally corresponded, meaning that the latter can be used as a proxy for the clinker 87Sr/86Sr isotope ratio. Finally, the concentrated hydrochloric acid/nitric acid dissolution method was found to be the most suitable sample preparation method for the cements; it is thus recommended for 87Sr/86Sr isotope analyses for cement provenancing.
KW - Cement
KW - Provenancing
KW - Sr isotopes
KW - Portland clinker
KW - Dissolution
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542239
DO - https://doi.org/10.1007/s00216-021-03821-7
SN - 1618-2642
SN - 1618-2650
VL - 414
IS - 15 (Topical collection: Analytical methods and applications in the materials and life sciences)
SP - 4379
EP - 4389
PB - Springer
CY - Berlin
AN - OPUS4-54223
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 - 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 - JOUR
A1 - Junge, Florian
A1 - Wittwer, Philipp
A1 - Sommerfeld, Thomas
A1 - Gehrenkemper, Lennart
A1 - Zoister, Christian
A1 - Nickl, Philip
A1 - Koch, Matthias
A1 - Meermann, Björn
A1 - Haag, Rainer
T1 - Adsorber Charge Dominates over Hydrophobic or Fluorophilic Functionalization in Influencing Adsorption of PFCA onto Polystyrene Resins
N2 - A systematic series of industrial-relevant polystyrene-based anion exchange resins that are functionalized with hydro- or fluorocarbon chains are compared regarding their adsorption behavior toward perfluorocarboxylic acids (PFCA) in respect to their charge, chain length, and type of chain. The results clearly show the dominance of electrostatic interactions in the adsorption process as uncharged adsorber materials showed no adsorption at all. In contrast, the charged adsorber materials showed in general a PFCA removal of 80% to 30% over the experiment depending on effluent fraction.
Unexpectedly, for perfluorobutanoic acid (PFBA) the highest removal rate is found with consistently >90%. Despite observing significant benefits in the adsorption of PFCA for fluoroalkylated adsorbers in comparison to their non-fluorinated counterparts, this effect of fluoroalkylation is comparatively small and can not be clearly attributed to fluorophilic interactions between the fluoroalkyl chains. These findings help clarifying that the introduction of fluorocarbon moieties in adsorber materials is not necessary in order to remove fluorocarbon molecules from the environment.
KW - PFAS
KW - Remediation
KW - Adsorption
KW - Fluorophilic interactions
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601883
DO - https://doi.org/10.1002/admi.202400199
SN - 2196-7350
SP - 1
EP - 10
PB - John Wiley & Sons
CY - Hoboken, New Jersey, USA
AN - OPUS4-60188
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fadda, Marta
A1 - Sacco, Alessio
A1 - Altmann, Korinna
A1 - Ciornii, Dmitri
A1 - Milczewski, Frank
A1 - Bañares, Miguel A.
A1 - Portela, Raquel
A1 - Giovannozzi, Andrea Mario
A1 - Rossi, Andrea Mario
T1 - Tracking nanoplastics in drinking water: a new frontier with the combination of dielectrophoresis and Raman spectroscopy
N2 - Detection of micro- (MPs) and nanoplastics (NPs) in food and environmental matrices has been gaining relevance due to their potential toxicological effects on human health. While MPs have been detected in a wide range of complex matrices, suitable methods for the characterization and chemical identification of NPs are still lacking, primarily due to significant methodological challenges associated with their nano-specific physiochemical properties, including size distribution (1 nm – 1 µm), dynamic surface chemical changes, and carbon-based composition, which complicate their detection compared to engineered nanomaterials. To overcome the traditional limitations of spectroscopic techniques in terms of spatial resolution and sensitivity at the sub-micrometer level, a novel label-free methodology is presented for specifically identifying the chemical composition of NPs directly in suspension by combining Raman spectroscopy with dielectrophoresis (DEP). Using a custom-built device, small volumes of NPs are injected into a dielectrophoretic cell and locally trapped by DEP forces to fill the Raman confocal volume, facilitating their detection and identification, and providing high signal-to-noise ratio Raman spectra for more reliable analysis. This approach was successfully applied to both Milli-Q water and a commercial brand of drinking water, enabling the rapid identification of various types of NPs with different sizes and polymer compositions at concentrations as low as 20 µg/mL. These included certified reference polystyrene beads ranging from 800 to 60 nm in diameter, as well as polydisperse NPs, more representative of real samples in terms of size distribution and polymer type, such as polyethylene (450 nm), polypropylene (180 nm), and polyethylene terephthalate (100 nm). Moreover, the chemical fingerprint of each NPs was thoroughly investigated and compared with the corresponding bulk polymers, highlighting possible changes in the Raman bands due to surface oxidation or nanometer-scale effect. Therefore, this innovative method can be considered a valuable approach for addressing gaps in the detection and identification of NPs, as well as for monitoring their dynamic phisiochemical changes in real matrices.
KW - Nanoplastics
KW - Water contaminants
KW - Raman microspectroscopy
KW - Dielectrophoresis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633658
DO - https://doi.org/10.1186/s43591-025-00131-y
SN - 2662-4966
VL - 5
IS - 1
SP - 1
EP - 11
PB - Springer Science and Business Media LLC
AN - OPUS4-63365
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Riedel, Soraya
A1 - Hülagü, Deniz
A1 - Bennet, Francesca
A1 - Carl, Peter
A1 - Flemig, Sabine
A1 - Schmid, Thomas
A1 - Schenk, J. A.
A1 - Hodoroaba, Vasile-Dan
A1 - Schneider, Rudolf
T1 - Electrochemical Immunomagnetic Ochratoxin A Sensing: Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine in Amperometric Assays
N2 - Electrochemical methods offer great promise in meeting the demand for user-friendly on-site devices for Monitoring important parameters. The food industry often runs own lab procedures, for example, for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with smart technologies. Enzyme-linked immunosorbent assays, with photometric detection of 3,3’,5,5’-tetramethylbenzidine (TMB),form a good basis for sensitive detection. To provide a straightforward approach for the miniaturization of the detectionstep, 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. A stable electrode response to TMB could be achieved at pH 1 on gold electrodes. We created a smartphonebased, electrochemical, immunomagnetic assay for the detection of ochratoxin A in real samples, providing a solid basis forsensing of further analytes.
KW - Ochratoxin A
KW - Amperometry
KW - Cyclic voltammetry
KW - Electrochemistry
KW - Immunoassay
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530421
DO - https://doi.org/10.1002/celc.202100446
N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S.
VL - 8
IS - 13
SP - 2597
EP - 2606
AN - OPUS4-53042
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Devi, Sarita
A1 - Riedel, Soraya
A1 - Döring, Sarah
A1 - Hiller, Lukas
A1 - Kaliyaraj Selva Kumar, Archana
A1 - Flemig, Sabine
A1 - Singh, Chandan
A1 - Konthur, Zoltán
A1 - Hodoroaba, Vasile-Dan
A1 - Schneider, Rudolf
T1 - Antibodies Functionalized Magnetic Fe-Metal-Organic Framework Based Biosensor for Electrochemical Detection of Tetanus Neurotoxin
N2 - This work presents a metal-organic framework (MOF)-integrated microfluidic flow-cell (MFC) based immunodetection of the tetanus toxoid (TT) using electrochemical technique for the first time. The magnetic property of Fe-MOF helped to hold them on the working electrode at detection zone of MFC surpassing the requirement of additional conjugation chemistry, whereas the conductive property was utilized to observe the change in signal efficiency in the presence of TT. The one-pot hydrothermal synthesis of a magnetic and conductive iron-based MOF (Fe-MOF) was performed using the Fe3 +/Fe2+ precursors as 1.2/1 mmol and dual ligands, i.e., tetrahydroxy-1,4-benzoquinone and 2-aminobenzene-1,4-dicarboxylic acid. The Fe-MOF was conjugated with L-phenylalanine (Fe-MOF/Phe) to increase its electric conductivity owing to the enhanced electron flow rate. The human monoclonal antibody SA13 against TT (anti-TT mAb) was conjugated on the Fe-MOF/Phe surface with the help of ethylenediamine (Fe-MOF/Phe/EDA/anti-TT mAb). The binding affinity of Fe-MOF/Phe/EDA/anti-TT mAb for the TT antigen was evaluated using cyclic voltammetry technique. The limit of detection of the Fe-MOF/Phe/EDA/anti-TT mAb-based biosensor for TT was 9.4 ng/ml in spiked buffer. This study shows the applicability of these Fe-MOFs in the detection of various other microbial toxins or other biomolecules.
KW - Antikörper
KW - Elektrochemischer Immunoassay
KW - Molecular Organic Framework (MOF)
KW - Microfluidics
KW - Rekombinant
PY - 2025
DO - https://doi.org/10.1016/j.snb.2025.137381
SN - 0925-4005
VL - 431
SP - 1
EP - 12
PB - Elsevier B.V.
CY - Amsterdam
AN - OPUS4-62673
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Bresch, Harald
A1 - Hodoroaba, Vasile-Dan
A1 - Schmidt, Alexandra
A1 - Rasmussen, K.
A1 - Rauscher, H.
T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice
N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory
requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials.
KW - Nano
KW - Particle size distribution
KW - Nanoparticle
KW - Nanomaterial
KW - OECD
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891
DO - https://doi.org/10.3390/nano12132238
SN - 2079-4991
VL - 12
IS - 13
SP - 2238
PB - MDPI
CY - Basel
AN - OPUS4-55189
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zia, Ghezal Ahmad Jan
A1 - Hanke, Thomas
A1 - Skrotzki, Birgit
A1 - Völker, Christoph
A1 - Bayerlein, Bernd
T1 - Enhancing Reproducibility in Precipitate Analysis: A FAIR Approach with Automated Dark-Field Transmission Electron Microscope Image Processing
N2 - AbstractHigh-strength aluminum alloys used in aerospace and automotive applications obtain their strength through precipitation hardening. Achieving the desired mechanical properties requires precise control over the nanometer-sized precipitates. However, the microstructure of these alloys changes over time due to aging, leading to a deterioration in strength. Typically, the size, number, and distribution of precipitates for a quantitative assessment of microstructural changes are determined by manual analysis, which is subjective and time-consuming. In our work, we introduce a progressive and automatable approach that enables a more efficient, objective, and reproducible analysis of precipitates. The method involves several sequential steps using an image repository containing dark-field transmission electron microscopy (DF-TEM) images depicting various aging states of an aluminum alloy. During the process, precipitation contours are generated and quantitatively evaluated, and the results are comprehensibly transferred into semantic data structures. The use and deployment of Jupyter Notebooks, along with the beneficial implementation of Semantic Web technologies, significantly enhances the reproducibility and comparability of the findings. This work serves as an exemplar of FAIR image and research data management.
KW - Industrial and Manufacturing Engineering
KW - General Materials Science
KW - Automated image analysis
KW - FAIR research data management
KW - Reproducibility
KW - microstructural changes
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593905
DO - https://doi.org/10.1007/s40192-023-00331-5
SN - 2193-9772
SP - 1
EP - 15
PB - Springer Science and Business Media LLC
CY - Heidelberg
AN - OPUS4-59390
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Alekseychuk, V. O.
A1 - Kupsch, Andreas
A1 - Plotzki, D.
A1 - Bellon, Carsten
A1 - Bruno, Giovanni
T1 - Simulation-Assisted Augmentation of Missing Wedge and Region-of-Interest Computed Tomography Data
N2 - This study reports a strategy to use sophisticated, realistic X-ray Computed Tomography (CT) simulations to reduce Missing Wedge (MW) and Region-of-Interest (RoI) artifacts in FBP (Filtered Back-Projection) reconstructions. A 3D model of the object is used to simulate the projections that include the missing information inside the MW and outside the RoI. Such information augments the experimental projections, thereby drastically improving the reconstruction results. An X-ray CT dataset of a selected object is modified to mimic various degrees of RoI and MW problems. The results are evaluated in comparison to a standard FBP reconstruction of the complete dataset. In all cases, the reconstruction quality is significantly improved. Small inclusions present in the scanned object are better localized and quantified. The proposed method has the potential to improve the results of any CT reconstruction algorithm.
KW - Computed tomography
KW - Missing wedge
KW - Region of interest
KW - Augmented data
KW - CT simulation
KW - aRTist
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593799
UR - https://www.mdpi.com/2313-433X/10/1/11
DO - https://doi.org/10.3390/jimaging10010011
SN - 2313-433X
VL - 10
IS - 1
SP - 1
EP - 15
PB - MDPI
CY - Basel
AN - OPUS4-59379
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Obenlüneschloß, Jorit
A1 - Boysen, Nils
A1 - Rönnby, Karl
A1 - Muriqi, Arbresha
A1 - Hoffmann, Volker
A1 - Abad Andrade, Carlos Enrique
A1 - Rogalla, Detlef
A1 - Brokmann, Ulrike
A1 - Rädlein, Edda
A1 - Nolan, Michael
A1 - Devi, Anjana
T1 - Rare Mononuclear Lithium-Carbene Complex for Atomic Layer Deposition of Lithium Containing Thin Films
N2 - Lithium is the core material of modern battery technologies and fabricating the lithium‐containing materials with atomic layer deposition (ALD) confers significant benefits in control of film composition and thickness. In this work, a new mononuclear N‐heterocyclic carbene (NHC) stabilized lithium complex, [Li(tBuNHC)(hmds)], is introduced as a promising precursor for ALD of lithium‐containing thin films. Structural characterization is performed, comparing density functional theory (DFT) and single‐crystal X‐ray diffraction (SC‐XRD), confirming a rare mononuclear structure. Favorable thermal properties for ALD applications are evidenced by thermogravimetric analysis (TGA). The compound exhibits a low melting point, clean evaporation, and its volatility parameters are encouraging compared to other lithium precursors. ALD trials using [Li(tBuNHC)(hmds)] with ozone demonstrate its effectiveness in depositing LiSixOy films. The ALD process exhibits a saturated growth per cycle (GPC) of 0.95 Å. Compositional analysis using Rutherford backscattering spectrometry/nuclear reaction analysis (RBS/NRA), X‐ray photoelectron spectrometry (XPS), and glow discharge optical emission spectrometry (GD‐OES), confirms the presence of lithium and silicon in the expected ratios. This work not only presents a new ALD precursor but also contributes to the understanding of lithium chemistry, offering insights into the intriguing coordination chemistry and thermal behavior of lithium complexes stabilized by NHC ligands.
KW - Atomic layer deposition (ALD)
KW - N-heterocyclic carbene (NHC) ligands
KW - Lithium ALD precursor chemistry
KW - Mononuclear Li–carbene complex [Li(tBuNHC)(hmds)]
KW - Li-silicate thin films (LiSixOy)
KW - Thermal properties & TGA/volatility
KW - Compositional analysis (RBS/NRA, XPS, GD-OES)
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643790
DO - https://doi.org/10.1002/anie.202513066
SN - 1433-7851
N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier
SP - 1
EP - 11
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-64379
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Danischewski, Julia L.
A1 - You, Yi
A1 - Bauer, Lauren
A1 - Riedel, Jens
A1 - Shelley, Jacob T.
T1 - Use of Resonant Acoustic Fields as Atmospheric-Pressure Ion Gates
N2 - Ion optics are crucial for spectrometric methods such as mass spectrometry (MS) and ion mobility spectrometry (IMS). Among the wide selection of ion optics, temporal ion gates are of particular importance for time-of-flight MS (TOF-MS) and drift-tube IMS. Commonly implemented as electrostatic ion gates, these optics offer a rapid, efficient means to block ion beams and form discrete ion packets for subsequent analysis. Unfortunately, these devices rely on pulsed high voltage sources and are not fully transparent, even in their open state, which can lead to ion losses and contamination. Here, a novel atmospheric-pressure ion gate based on a resonant acoustic field structure is described. This effect was accomplished through the formation of a resonant, standing acoustic wave of alternating nodes and antinodes. Alignment of an atmospheric-pressure gaseous ion beam with an antinode, i.e. a region of transient pressure, of the acoustic structure acted as a gate and blocked ions from impinging on ion-selective detectors, such as a mass spectrometer and a Faraday plate. The velocity of the ion stream and acoustic power were found to be critical parameters for gating efficiency. In the presence of an acoustic field (i.e., a closed gate), ion signals decreased by as much as 99.8% with a response time faster than the readout of the ion-measurement devices used here (ca. 75 ms). This work demonstrates the basis for a low-cost, acoustic ion gate, which is optically transparent and easily constructed with low-power, off-the-shelf components, that could potentially be used with MS and IMS instrumentation.
KW - Acoustic Ion Manipulation
PY - 2025
DO - https://doi.org/10.1021/acs.analchem.4c05493
SN - 1520-6882
VL - 97
IS - 5
SP - 2890
EP - 2898
PB - American Chemical Society
AN - OPUS4-62648
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Onyenso, Gabriel
A1 - AI-Zawity, Jiwar
A1 - Farahbakhsh, Nastaran
A1 - Schardt, Annika
A1 - Yadigarli, Aydan
A1 - Vakamulla Raghu, Swathi Naidu
A1 - Engelhard, Carsten
A1 - Müller, Mareike
A1 - Schönherr, Holger
A1 - Killian, Manuela S.
T1 - Novel Ag-modified zirconia nanomaterials with antibacterial activity
N2 - The outcome of an implant procedure largely depends on the implant's surface properties. Biomaterials are now designed to have surfaces with multifunctionality, such as favorable tissue integration and the ability to combat bacterial adhesion and colonization. Herein, we report on a simple approach to improve the antibacterial properties of zirconia nanotubes (ZrNTs) coatings by decorating with silver nanoparticles (AgNP), achieved through electrochemical anodization of a zirconium–silver alloy (Zr–Ag). The AgNPs were shown to partially consist of Ag2O, potentially enhancing the availability of Ag+ ions for antibacterial activity. The modified ZrNTs were characterized using SEM, EDS, ToF-SIMS, and XPS to determine their structural morphology and chemical composition, and were further subjected to antibacterial testing. The silver and zirconium ion release behavior was monitored via ICP-MS. ZrNTs decorated with AgNP exhibit strong antimicrobial activity (>99% bacterial killing) against both S. aureus and E. coli. Antimicrobial tests indicate that the antibacterial activity against the Gram-positive pathogen S. aureus was improved by a factor of 100 compared to unmodified ZrNTs, while unmodified ZrNTs already showed a comparable reduction of viable Gram-negative E. coli. This strategy illustrates a straightforward and effective modification that optimizes the interface between the host environment and the biomaterial surface to meet the very important criteria of biocompatibility and active antibacterial response.
KW - Mass Spectrometry
KW - Nanoparticles
KW - Advanced Materials
KW - ICP-MS
KW - Antimicrobial material
KW - ToF-SIMS
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653990
DO - https://doi.org/10.1039/d5ra07099f
SN - 2046-2069
VL - 16
IS - 3
SP - 2286
EP - 2297
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65399
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Putzu, Mara
A1 - Wiesner, Yosri
A1 - Weimann, Christiane
A1 - Hodoroaba, Vasile-Dan
A1 - Muniategui Lorenzo, Soledad
A1 - Fernández-Gonzáles, Verónica
A1 - Booth, Andy M.
A1 - Igartua, Amaia
A1 - Benismail, Nizar
A1 - Coïc, Laureen
A1 - Chivas-Joly, Carine
A1 - Fenoglio, Ivana
A1 - Rossi, Andrea Mario
A1 - Giovannozzi, Andrea Mario
A1 - Altmann, Korinna
T1 - Optimization of tablet processing as a reference material for microplastic detection methods
N2 - Reference materials (RMs) are essential and highly demanded tools for the development and validation of methods for microplastic (MP) quantification in complex matrices, to ensure comparable and harmonized approaches aligned with EU commission criteria for monitoring MPs (e.g., Drinking Water Directive and Urban Wastewater Treatment Directive). This study investigates different approaches for optimizing the production of polypropylene (PP) RMs in the form of water-soluble tablets, which were carefully evaluated for their homogeneity and stability according to ISO Guide 30, ISO 33401, and ISO 33405. PP particles (1–100 μm) were produced by cryomilling and embedded in a lactose/PEG matrix, then pressed into tablets (18 µg theoretical PP mass). The production process was optimized by varying (i) the size distribution of the matrix components and (ii) the mixer instrument. The materials obtained were characterized by thermogravimetric analysis to assess the homogeneity distribution of MPs with respect to PP mass in the individual tablets and their stability over a 4-month period. The most promising approach, with a homogenous mass of 19 μg (standard deviation of 4 μg), relative standard deviation of 19%, was further investigated for homogeneity by comparison with thermo-analytical mass determination methods, such as TED-GC/MS (thermal extraction desorption-gas chromatography/mass spectrometry) and Py-GC/MS (pyrolysis-gas chromatography-mass spectrometry), and for number-based characterization using micro-Raman spectroscopy. Material characterization was also examined using laser diffraction, scanning electron microscopy, and ATR-FTIR. Based on the results, the optimized processing protocol yields a PP RM suitable for quality control and method performance studies supporting standardization.
KW - Microplastics
KW - TED-GC/MS
KW - Reference materials
KW - Polypropylene
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653290
DO - https://doi.org/10.1007/s00216-025-06271-7
SN - 1618-2642
SP - 1
EP - 14
PB - Springer Science and Business Media LLC
AN - OPUS4-65329
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Li, Xunyu
A1 - Riedel, Jens
A1 - You, Yi
T1 - Practical high-resolution spectroscopy with a spatial heterodyne spectrometer: Determination of instrumental function for lineshape recovery
N2 - The spatial heterodyne spectrometer (SHS) is a well-recognized platform for its high resolving power in various use cases of spectroscopy. Same as other spectrometer topologies, the SHS, unfortunately, also suffers from classical challenges such as distorted lineshape due to the instrumental function. The goal of this work is to tackle this persisting issue through a simple numerical approach. With the inherent characteristics of an SHS interferogram, we report the direct extraction and determination of the instrumental function in its numerical representation from an SHS interferogram; this instrumental function was further used for spectral data processing that enables significant improvements in spectral resolution through deconvolution algorithms.Here, we systematically discuss the recognition of the embedded instrumental function among various ingredients within an interferogram. To verify the numerical approach, lithium was chosen as the model sample, resembling the use of SHS in an isotopic analysis application. Specifically, the resonance transition of lithium D-lines (2P1/2,3/2 ← 2S1/2) was selected to assess the performance of the spectral processing. With the spectral deconvolution, the spectral features that represent the 6Li and 7Li were nearly baseline-separated, allowing for the accurate measure of the isotopic abundance without external references or algorithm adjustments (e.g., curve fitting).
KW - SHS
KW - Isotopic analysis
KW - High Resolution
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613401
DO - https://doi.org/10.1016/j.sab.2024.107053
SN - 0584-8547
VL - 221
SP - 1
EP - 5
PB - Elsevier
AN - OPUS4-61340
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Steinbeck, Christoph
A1 - Jung, Nicole
A1 - Bach, Felix
A1 - Neumann, Steffen
A1 - Herres-Pawlis, Sonja
A1 - Liermann, Johannes
A1 - Koepler, Oliver
A1 - Bannwarth, Christoph
A1 - Bender, Theo
A1 - Bocklitz, Thomas
A1 - Boehm, Franziska
A1 - Bonatto Minella, Christian
A1 - Biedermann, Frank
A1 - Brack, Werner
A1 - Cunha, Ricardo
A1 - Czodrowski, Paul
A1 - Eberl, Franziska
A1 - Engel, Thomas
A1 - Engstfeld, Albert
A1 - Fischer, Tillmann G.
A1 - Friedrich, Pascal
A1 - Glorious, Frank
A1 - Golub, Benjamin
A1 - Grathwol, Christoph
A1 - Haag, Rainer
A1 - Hunold, Johannes
A1 - Jacob, Christoph
A1 - Johannsen, Jochen
A1 - Jollife, John
A1 - Kast, Stefan
A1 - Kettner, Carsten
A1 - Kuhn, Stefan
A1 - Lanza, Giacomo
A1 - Lisec, Jan
A1 - Manolikakes, Georg
A1 - Mata, Ricardo
A1 - Meiler, Jens
A1 - Müller, Matthias
A1 - Müller-Pfefferkorn, Ralph
A1 - Ortmeyer, Jochen
A1 - Patterson, Wendy
A1 - Pleiss, Jürgen
A1 - Riedel, Annalisa
A1 - Riedel, Jens
A1 - Schatzschneider, Ulrich
A1 - Schuster, Leonie
A1 - Seeberger, Peter
A1 - Seibert, Johann-Nikolaus
A1 - Stadler, Peter
A1 - Zeitler, Kirsten
T1 - Proposal NFDI4Chem 2025-2030 In the National Research Data Infrastructure (NFDI) — Our Vision: All Chemists Publish FAIR Data
N2 - The first funding period of NFDI4Chem established a robust foundation for research data management (RDM) in chemistry by promoting FAIR data principles and creating a cohesive infrastructure to capture well-annotated data early in the lab through electronic lab notebooks (ELNs) and making this data available in public repositories. Key achievements include standardised data formats and metadata, a federated repository environment, and improved data visibility and accessibility. Training programs and outreach have significantly increased awareness and adoption of best RDM practices. In the second funding period, the consortium aims to advance these achievements by consolidating this infrastructure, developing a model for its sustainable maintenance and operation, and fostering cultural change for its widespread adoption. Goals include ensuring seamless data workflows from laboratories to open repositories, enhancing interoperability, and supporting innovative research through AI-ready data. The work plan is organised into six task areas (TAs). TA1 (Management) provides leadership and supports all other TAs in achieving their objectives. TA2 (Smart Lab) aims to develop a fully digital research environment, including an ELN as a modular platform. This environment will support data collection, management, storage, analysis, and sharing. Integrating devices and external resources will enable seamless data transfer to repositories. TA3 (Repositories) will consolidate the repository ecosystem. The goal is to integrate repositories into a federated system for better accessibility and interoperability, ensuring long-term data availability and sustainability. TA4 (Metadata, Data Standards, and Publication Standards) focuses on developing and promoting new data and metadata standards in an international community process. This includes applying ontologies to create a semantic foundation for linking research data, making it machine-readable and enabling knowledge graphs. TA5 (Community and Training) is dedicated to fostering a cultural shift towards digital chemistry through continuous engagement, collecting requirements, and providing extensive training and support through workshops and open education resources. It will promote FAIR-compliant machine learning applications, embedding RDM into academic curricula to ensure future scientists are well-versed in these practices. TA6 (Synergies and Cross-Cutting Topics) aims to enhance collaboration across NFDI consortia and beyond. This includes developing ontologies, terminology services, the search service, and other cross-cutting solutions, integrating these developments into existing infrastructure, enabling interdisciplinary data harmonisation and fostering machine learning applications.
KW - Research Data Management
KW - FAIR
KW - Chemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648540
DO - https://doi.org/10.3897/rio.11.e177037
SN - 2367-7163
VL - 11
SP - 1
EP - 100
PB - Pensoft Publishers
AN - OPUS4-64854
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - You, Yi
A1 - Danischewski, Julia
A1 - Molnar, Brian
A1 - Riedel, Jens
A1 - Shelley, Jacob
T1 - Manipulation of Gaseous Ions with Acoustic Fields at Atmospheric Pressure
N2 - The ability to controllably move gaseous ions is an essential aspect of ion-based spectrometry (e.g., mass spectrometry and ion mobility spectrometry) as well as materials processing. At higher pressures, ion motion is largely governed by diffusion and multiple collisions with neutral gas molecules. Thus, high-pressure ion optics based on electrostatics require large fields, radio frequency drives, complicated geometries, and/or partially transmissive grids that become contaminated. Here, we demonstrate that low-power standing acoustic waves can be used to guide, block, focus, and separate beams of ions akin to electrostatic ion optics. Ions preferentially travel through the static-pressure regions (“nodes”) while neutral gas does not appear to be impacted by the acoustic field structure and continues along a straight trajectory. This acoustic ion manipulation (AIM) approach has broad implications for ion manipulation techniques at high pressure, while expanding our fundamental understanding of the behavior of ions in gases.
KW - Ion mobility spectrometry
KW - Acoustic
KW - Mass spectrometry
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600704
DO - https://doi.org/10.1021/jacs.4c01224
SP - 1
EP - 6
PB - ACS Publications
AN - OPUS4-60070
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - van Wasen, S.
A1 - You, Yi
A1 - Beck, S.
A1 - Riedel, Jens
A1 - Volmer, D. A.
T1 - Laser Ablation Secondary Electrospray Ionization for In Situ Mass Spectrometric Interrogation of Acoustically-Levitated Droplets
N2 - The composition of acoustically levitated droplets was probed by a novel combination of mid-IR laser evaporation and subsequent postionization via secondary electrospray ionization. The combination of microliter samples and subnanoliter sampling provided time-resolved interrogation of droplets and allowed for a kinetic investigation of the laser-induced release of the analyte, which was found to strongly depend on the analytes. The observed substancespecific delayed release of the analytes permitted baseline-separated discrimination of the analytes, ideal for the study of complex samples.
The additionally applied postionization scheme was found to enable efficient detection of small volatile compounds as well as peptides. The detection of small molecules and peptides occurred under very different sampling geometries, pointing to two distinct underlying ionization mechanisms. Overall, our results suggest that the experimental setup presented in this study can serve as a widely applicable platform to study chemical reactions in acoustically levitated droplets as model reactors.
KW - Acoustic levitation
KW - Mass spectrometry
KW - Electrospray
KW - Laser ablation
PY - 2022
DO - https://doi.org/10.1021/acs.analchem.2c03800
SN - 0003-2700
VL - 2022
SP - 1
EP - 5
PB - ACS Publications
CY - Washington
AN - OPUS4-56531
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Xue, Boyang
A1 - Wang, Zhangjun
A1 - Zhu, Tao
A1 - Gu, Yezhen
A1 - Sun, Weihong
A1 - Chen, Chao
A1 - Li, Zhigang
A1 - Riedel, Jens
A1 - You, Yi
T1 - High repetition-rate laser-induced breakdown spectroscopy combined with two-dimensional correlation method for analysis of sea-salt aerosols
N2 - Laser-induced breakdown spectroscopy (LIBS) offers a tantalizing glimpse into real-time, on-the-spot aerosol analysis. Yet, the reliance on traditional lasers, with their limitations in energy and frequency, hampers optimal sample handling, dissociation, and excitation. To address those challenges, we propose a novel tactic: utilize a high repetition-rate (rep.-rate) laser with low pulse energy in combination with the two-dimensional correlation (2D-corr.) technique for sea-salt aerosols analyses. By examining the emission patterns from both the laser pulse train and individual pulses, we recognize distinctive analyte-specific rep.-rate responses, which allowed spectral reconstruction of analytes, avoiding background interferences. This discovery enabled the rep.-rate modulation for a 2D-corr. spectroscopy workflow. Consequently, we successfully differentiated between particle-related and air-species-related spectral components, obviating expensive spectrometers or intensified image detectors. For instance, the Na I at 589 nm stemming from aerosols exhibited an entirely different correlation contribution compared to O I at 777 nm, resulting in reconstructed clean aerosol-spectra without spectral peaks originated from air species. This 2D-corr. aerosol LIBS approach shows promising analytical potential streamlining aerosol particle analysis.
KW - LIBS
KW - Aerosol
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613392
DO - https://doi.org/10.1016/j.sab.2024.107048
SN - 0584-8547
VL - 221
SP - 1
EP - 8
PB - Elsevier
AN - OPUS4-61339
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Li, Xunyu
A1 - Riedel, Jens
A1 - You, Yi
T1 - Spectrally resolved lithium isotope quantification through high-resolution spatial heterodyne spectrometry
N2 - Isotope ratio determination of lithium is increasingly important in fields ranging from geochemistry to battery diagnostics. While mass spectrometry remains the gold standard, it is costly, cumbersome, and incompatible with portable or inline implementations. Optical emission spectroscopy presents an appealing alternative. However, it is traditionally limited by insufficient spectral resolution or resolving power to separate lithium isotope emissions due to their generalized designs for a wide spectral range; this often requires overly complicated algorithms to overcome the instrumental drawbacks. (79)
Results Here, we report a high-resolution optical method for lithium isotope quantification using a custom-built spatial heterodyne spectrometer (SHS) combined with a reduced-pressure glow discharge source. This configuration yielded a resolving power of 189,000 and enabled baseline resolution of lithium d-line emission features even without the need for preliminary data processing. Despite the inherent low sensitivity of SHS, a detection limit of 30 pmol was achieved using a standard industrial camera. To improve quantitative accuracy, we introduced a deconvolution-based spectral lineshape recovery technique alongside a bootstrapping-based error propagation strategy. These methods facilitated robust isotope ratio calibration using both peak-height and peak-area metrics. The SHS platform additionally enabled the determination of relative transition probabilities, suggesting the feasibility of calibration-free operation.
This work demonstrates the practical viability of SHS for high-specificity, high-resolution lithium isotope analysis. The approach is compact, potentially field-deployable, and adaptable to other elements with optically resolvable isotope shifts, offering a route toward accessible and calibration-free optical isotopic analyses.
KW - SHS
KW - Isotope
KW - High-resolution spectroscopy
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635139
DO - https://doi.org/10.1016/j.aca.2025.344329
SN - 1873-4324
VL - 1368
SP - 1
EP - 8
PB - Elsevier B.V.
AN - OPUS4-63513
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mohan, M.
A1 - Prochazka, D.
A1 - You, Yi
A1 - Riedel, Jens
A1 - Gornushkin, Igor
A1 - Rocnakova, I.
A1 - Papula, M.
A1 - Porízka, P.
A1 - Kaizer, J.
T1 - Investigating plasma morphology at material boundaries under varying ambient pressures
N2 - Laser-Induced Breakdown Spectroscopy (LIBS) is a widely used technique for elemental analysis. The analysis of the obtained LIBS spectra generally assumes plasma homogeneity. However, using focused laser beams for interrogation, LIBS probes materials on the microscale and is, thus, prone to artefacts from sample heterogeneities on the micrometer scale. An ablation at a material boundary of two matrices may result in a significant inhomogeneity in the plasma plume, which can severely impact the accuracy of quantitative analysis. Since this propagation of the surface morphology into the plasma plume is driven by the plasma expansion, its final impact is strongly pressure dependent. This study examines the influence of varying ambient pressures (7–1000 mbar) on plasma morphology, spectral characteristics, and key plasma properties such as electron number density at a well-defined Cu–Sn boundary, in comparison with the results obtained using homogeneous alloys. Several approaches of plasma imaging with bandpass filters, spectroscopy, and Radon transform-based 3D reconstruction were employed to analyze elemental distribution, signal-to-noise (SNR) and signal-to-background (SBR) ratios, as well as electron number densities. The 3D reconstructions revealed a pronounced plasma asymmetry for the ablation at the material boundary, in contrast to the near-axial symmetry observed for the ablation of homogeneous alloys. At lower pressures, this distinct elemental separation in plasma persisted, while higher pressures led to an increased collisional mixing and homogenization. SNR and SBR were consistently lower for ablation at the boundary compared to homogeneous samples. These findings highlight how boundary ablation contributes to plasma inhomogeneities in LIBS analysis of heterogeneous materials and emphasize the need to account for these
effects when using LIBS for elemental mapping of fine heterogeneous structures.
KW - Laser-induced breakdown spectroscopy
KW - Plasma inhomogeneity
KW - Plasma tomography
KW - Radon transform
KW - Material boundaries
KW - Ambient pressure effects
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634777
DO - https://doi.org/10.1016/j.talanta.2025.128377
SN - 1873-3573
VL - 295
SP - 1
EP - 8
PB - Elsevier B.V.
AN - OPUS4-63477
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - You, Yi
A1 - Xue, Boyang
A1 - Riedel, Jens
T1 - Enhancement of LIBS plasma in air with organic solvent vapors
N2 - Laser-induced breakdown spectroscopy (LIBS) offers versatile, field-deployable elemental analysis; however, compact, high-repetition-rate nanosecond laser systems typically face constraints in power consumption and size, often compromising emission intensity and thus analytical performance. We demonstrate a significant improvement in LIBS signals through the controlled introduction of common organic solvent vapors into a sheath gas, with a diode-pumped solid-state laser (1064 nm, 2–28 kHz repetition rate, 450–600-μJ pulse energy). Optical and acoustic diagnostics reveal up to ca. 40-fold enhancement of the N II emission line at 567 nm when ambient air serves as the analyte. Maximal enhancement occurs at intermediate repetition rates of ca. 15 kHz, particularly at pulse energies approaching the optical breakdown threshold; this observation suggests a viable strategy for operating LIBS at lower pulse energies and higher repetition rates. Enhancement effects scale jointly with both vapor pressure and ionization energy of the organic species, with acetone and toluene markedly outperforming methanol and isopropanol. These findings provide a rational foundation for significantly improving the analytical performance of portable LIBS instruments without exceeding platform-specific constraints.
KW - LIBS
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653758
DO - https://doi.org/10.1016/j.sab.2025.107309
SN - 0584-8547
VL - 236
SP - 1
EP - 6
PB - Elsevier B.V.
AN - OPUS4-65375
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wittwer, Philipp
A1 - Roesch, Philipp
A1 - Vogel, Christian
A1 - Simon, Fabian
A1 - Gehrenkemper, Lennart
A1 - Feldmann, Ines
A1 - Simon, Franz-Georg
T1 - Less Is More: Influence of Cross-Linking Agent Concentration on PFOS Adsorption in Chitosan
N2 - As a result of the continuous use of persistent per- and polyfluoroalkyl substances (PFAS), e.g., in aviation firefighting foams, contamination with PFAS has been found in soil, groundwater, and surface water around thousands of industrial and military installations. Due to their harmful (environmental) potential, further dispersion in the environment needs to be stopped, which can be achieved by appropriate absorption materials. In this work, the influence of the cross-linking agent epichlorohydrin (ECH) concentration on the perfluorooctanesulfonic acid (PFOS) adsorption capacity of chitosan gel was investigated. It was found that higher ECH concentration during the cross-linking step decreases the PFOS adsorption capacity of the cross-linked chitosan gel from 0% to 4% ECH solution by about 15%. Using a concentration of 1%, ECH resulted still in an acid-stable material, and a maximum PFOS loading capacity of 4.04 mmol/g was obtained, one of the highest described in the literature. Furthermore, we used a rapid small-scale column test to compare the PFOS adsorption capacity of chitosan and activated carbon, each in both milled and unmilled form. Unmilled chitosan showed the highest PFOS adsorption capacity considering adsorption material dry masses (>0.9 and <0.4 mmol/g for both types of chitosan and activated carbon, respectively). Milled activated carbon proved to be the better adsorption material, considering the fixed volume of the adsorber (>99.9% PFOS adsorbed). Overall, the cross-linking agent concentration in chitosan is a crucial factor influencing its PFOS absorption potential. Our results feature cross-linked chitosan as an effective economic and ecologic alternative for PFOS adsorption in aqueous solutions.
KW - Combustion Ion Chromatography
KW - Per- and Polyfluoroalkyl substances (PFAS)
KW - Remediation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618406
DO - https://doi.org/10.3390/app142311145
VL - 14
IS - 23
SP - 1
EP - 13
PB - MDPI
AN - OPUS4-61840
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Vogel, Christian
A1 - Urban, Klaus
A1 - Ackerhans, C.
A1 - Gorbushina, Anna
T1 - Analysis of Carbon and Nitrogen from Atmospheric Sources by Bulk Deposition Sampling at various locations in Germany
N2 - Atmospheric deposition of particulate matter is an important indicator of air pollution and a significant factor in material surface fouling. The elemental composition of this nutrient-containing dust depends largely on the exposure region and time as well as on climate. Therefore, in this paper we report an analysis of atmospheric pollutions with a self-made low-cost bulk deposition sampler directed at sampling deposition via air transport and rainfall. We used the device in diverse environments - thus comparing an urban region, an area surrounded by forest and an area mainly dominated by agriculture. The total organic carbon (TOC) and total nitrogen (TN) amounts were selected as indicator parameters and analyzed in a biweekly rhythm for three and a half and two years, respectively. The TOC value responded to particulate matter in the urban area, especially significant were the influences of the New Year's firework in urban and pollen in the rural forest area. In contrast, the TN value was more under the influence of the nitrogen emissions in the agriculture-dominated area. However, the TN value did not correlate with the NOx values in the urban area because the atmospheric nitrogen emissions in the city might originate from various emission sources. Summarizing, the TOC and TN values of the self-made low-cost bulk deposition sampler were in good agreement with environmental events of their immediate surrounding. Moreover, the selected containers and sampling procedures are universally applicable to monitor and analyze organic as well as inorganic parameters (e.g. metal ions) of atmospheric deposition.
KW - Passive sampling
KW - Biomonitoring
KW - Air Analysis
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609373
DO - https://doi.org/10.1016/j.envadv.2024.100583
SN - 2666-7657
VL - 17
SP - 1
EP - 9
PB - Elsevier Ltd.
AN - OPUS4-60937
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 - 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 -
TY - JOUR
A1 - Weidner, Steffen
A1 - Meyer, A.
A1 - Kricheldorf, H.
T1 - Transformation of poly(L-lactide) crystals composed of linear chains into crystals composed of cycles
N2 - A poly(L-lactide) with a trifluoroethyl ester end group and an average degree of polymerization (DP) of 50 was synthesized by ROP of L-lactide initiated with trifluoroethanol. Small-angle X-ray scattering (SAXS) in combination with differential scanning calorimetry (DSC) measurements revealed an average crystal thickness of 13 nm, corresponding to 45 repeat units. This suggests that most crystallites were formed by extended PLA chains, and both flat surfaces were covered by CF3 groups. The crystalline PLAs were annealed at 140 or 160 °C in the presence of two catalysts: tin(II) 2-ethylhexanoate, (SnOct2) or dibutyltin bis(pentafluorophenoxide) (BuSnPhF). The chemical reactions, such as polycondensation and cyclization, proceeded in the solid state and were monitored by matrix-assisted laser desorption/ionization time-offlight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC) measurements. Under optimal conditions a large fraction of linear chains was transformed into crystallites composed of extended cycles. Additionally, MALDI TOF MS analysis of GPC fractions from samples annealed for 28 or 42 days detected chain elongation of the linear species up to a factor of 20.
KW - Polylactide
KW - MALDI-TOF MS
KW - Crystalinity
KW - Transesterification
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597250
DO - https://doi.org/10.1039/D3PY01370G
SN - 1759-9954
VL - 15
IS - 12
SP - 1173
EP - 1181
PB - Royal Society for Chemistry
AN - OPUS4-59725
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -