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Paper des Monats
- ja (27)
X-ray scattering datasets for samples described in the 2022 publication "Molecular Mobility of Polynorbornenes with Trimethylsiloxysilyl side groups: Influence of the Polymerization Mechanism". This dataset includes both raw and processed X-ray scattering data for samples APTCN and MPTCN, alongside background measurements files (BKG).
X-ray scattering datasets for samples described in the 2020 publication "Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation". This dataset includes both raw and processed X-ray scattering data for samples PTCHSiO-Pr, Bu, Hx, Oc and De, alongside background measurements files (BKG). This data was collected using the MOUSE project (instrument and methodology).
Reclaimed asphalt pavements (RAP) with increased contents of polycyclic aromatic hydrocarbons (PAH) are restricted for reuse due to their harmful effects on humans and the environment. This work investigated whether Fourier transform infrared (FTIR) spectroscopy is suitable for a fast and simple identification and quantification of PAH in binders recovered from reclaimed asphalts. For this, the binders from 34 RAP samples were recovered using a rapid procedure developed at the Universität Kassel and were examined with infrared spectroscopy. The obtained spectra were pre-processed (Standard Normal Variate transformation, 1st derivative) and evaluated using a combination of factor analysis and linear discriminant analysis. The results showed that various PAH groups with differently pronounced aromatic structures are present in the binders.
However, with FTIR spectroscopy combined with the multivariate methods, a statistical model was developed allowing for the differentiation between the PAH groups and also for the distinction between PAH contents below or above the threshold of 25 mg/kg valid in Germany.
Large, ink-bottle-shaped pores in mesocellular foams (MCFs) are desired for various applications requiring enhanced mass transfer or the immobilization of larger compounds. Hence, the cylindrical pores of COK-12, an ordered mesoporous silica structurally comparable to SBA-15 but synthesized at room-temperature at quasi-neutral pH, are chemically swollen into ink-bottle pores. Therefore, p-xylene is used as a more sustainable swelling agent compared to popular alternatives. Its high boiling point allows for an additional thermal aging step to amplify the mesostructure enlargement without needing additional chemicals. For COK-12, the MCFs obtained at room temperature reach an unprecedented plateau for the modal mesopore cell and window diameter of 19.9 and 5.5 nm, respectively, with an underlying broad pore size distribution and distorted hexagonal lattice up to 14.5 nm, involving hexagonal and spherical structures. The combined chemical and thermal swelling resulted in the selective enlargement of the window diameter to more than 200% and a slightly increased cell diameter, pore size distribution, and hexagonal lattice distortion in comparison to the room temperature synthesis. Such materials are thought to be promising alternatives to SBA-15-based MCFs, often utilizing toxic catalysts during synthesis. The presented results pave the way for enhanced adsorptive, catalytic, and drug delivery performances for COK-12-based materials.
Decades of non-destructive evaluation (NDE) for the quality assurance of concrete bridges revealed the necessity of developing procedures for building reference specimens for different defects. External objects have been widely used in specimen construction to represent defects. However, embedded materials can alter the actual defect characteristics, interrupting the NDE responses. This study proposes new approaches to fabricating reference specimens for reinforced concrete that feature substantial defects, including cracks, delamination, honeycombing and rebar corrosion, without external objects. As a result, realistic responses can be acquired to identify promising NDE methods for characterising actual deteriorations. The procedures were produced with the intent of being reproducible in any laboratory. Destructive and non-destructive testing methods were performed to verify the effectiveness of the processes in creating defects. This study provides research laboratories with techniques for
fabricating reference specimens for characterising defects and assessing the performance of NDE technologies.
Despite their inherent instability, 4n π systems have recently received significant attention due to their unique optical and electronic properties. In dibenzopentalene (DBP), benzanellation stabilizes the highly antiaromatic pentalene core, without compromising its amphoteric redox behavior or small HOMO−LUMO energy gap. However, incorporating such molecules in organic devices as discrete small molecules or amorphous polymers can limit the performance (e.g., due to solubility in the battery electrolyte solution or low internal surface area). Covalent organic frameworks (COFs), on the contrary, are highly ordered, porous, and crystalline materials that can provide a platform to align molecules with specific properties in a well-defined, ordered environment. We synthesized the first antiaromatic framework materials and obtained a series of three highly crystalline and porous COFs based on DBP. Potential applications of such antiaromatic bulk materials were explored: COF films show a conductivity of 4 × 10−8 S cm−1 upon doping and exhibit photoconductivity upon irradiation with visible light. Application as positive electrode materials in Li-organic batteries demonstrates a significant enhancement of performance when the antiaromaticity of the DBP unit in the COF is exploited in its redox activity with a discharge capacity of 26 mA h g−1 at a potential of 3.9 V vs. Li/Li+ . This work showcases antiaromaticity as a new design principle for functional framework materials.
Air-coupled ultrasound sensors have advantages over contact ultrasound sensors when a sample should not become contaminated or influenced by the couplant or the measurement has to be a fast and automated inline process. Thereby, air-coupled transducers must emit high-energy pulses due to the low air-to-solid power transmission ratios (10−3 to 10−8). Currently used resonant transducers trade bandwidth—a prerequisite for material parameter analysis—against pulse energy. Here we show that a combination of a non-resonant ultrasound emitter and a non-resonant detector enables the generation and detection of pulses that are both high in amplitude (130 dB) and bandwidth (2 µs pulse width). We further show an initial application: the detection of reflections inside of a carbon fiber reinforced plastic plate with thicknesses between 1.7 mm and 10 mm. As the sensors work contact-free, the time of flight and the period of the in-plate reflections are independent parameters. Hence, a variation of ultrasound velocity is distinguishable from a variation of plate thickness and both properties are determined simultaneously. The sensor combination is likely to find numerous industrial applications necessitating high automation capacity and opens possibilities for air-coupled, single-side ultrasonic inspection.
A solvothermal method was used to prepare a series of Yb3+/Tm3+/Ca2+ co-doped NaYF4 nanoparticles with different Ca2+ contents. Strong upconversion blue fluorescence could be observed under 980 nm laser excitation of the samples. The effect of different Ca2+ contents on the luminescence intensity was investigated, and it was found that the UV-vis upconversion luminescence increased and then decreased with an increasing Ca2+ concentration during the increase of the Ca2+ content from 0 mol% to 25 mol%, reaching the strongest fluorescence at 15 mol%, which was up to about 28 times stronger than that without Ca2+ doping. Furthermore, the mechanism was investigated, and it was found that the doping of Ca2+ disrupted the symmetry of the crystal field, resulting in a significant enhancement of the overall fluorescence. Applied to fluorescence intensity ratio thermometry, the absolute and relative sensitivities are as high as 0.0418 K−1 and 2.31% K−1, respectively, with a minimum temperature resolution of 0.0129 K.
Etalon features in transmittance spectra of films arise due to the coherent superposition of waves caused by reflections multiple times at the inner film boundaries. The fringe maxima occur at i𝜆 = 2nd cos 𝜑 with i - being an integer, 𝜆 - the wavelength, d - the film thickness, 𝜑 - the angle of incidence in respect to the film normal and n - the refractive index of the film. It is obvious that such features can hinder the interpretation of absorption bands when fringe amplitude and period are in the same range as the expected bands.
This poster discusses the suitability of two optical methods for the THz spectral range applied to Fourier Transform Spectroscopy.
Etalon effects in THz transmittance spectra, either taken in time- domain or frequency-domain, often hamper or even hinder the interpretation of film properties. In this paper we discuss the transferability and applicability of spectroscopic methods typically employed in the near and mid infrared spectral range to eliminate the fringes in the transmittance spectra in the THz spectral range.
Cryoadsorption on the inner surface of porous materials is a promising solution for safe, fast, and reversible hydrogen storage. Within the class of highly porous metal−organic frameworks, zeolitic imidazolate frameworks (ZIFs) show high thermal, chemical, and mechanical stability. In this study, we selected ZIF-8 synthesized mechanochemically by twin-screw extrusion as powder and pellets. The hydrogen storage capacity at 77 K and up to 100 bar has been analyzed in two laboratories applying three different measurement setups showing a high reproducibility. Pelletizing ZIF-8 increases the packing density close to the corresponding value for a single crystal without loss of porosity, resulting in an improved volumetric hydrogen storage capacity close to the upper limit for a single crystal. The high volumetric uptake combined with a low and constant heat of adsorption provides ca. 31 g of usable hydrogen per liter of pellet assuming a temperature−pressure swing adsorption process between 77 K − 100 bar and 117 K − 5 bar. Cycling experiments do not indicate any degradation in storage capacity. The excellent stability during preparation, handling, and operation of ZIF-8 pellets demonstrates its potential as a robust adsorbent material for technical application in pilot- and full-scale adsorption vessel prototypes.
The 18O/16O ratio of cherts (δ18Ochert) increases nearly monotonically by ~15‰ from the Archean to present. Two end-member explanations have emerged: cooling seawater temperature (TSW) and increasing seawater δ18O (δ18Osw). Yet despite decades of work, there is no consensus, leading some to view the δ18Ochert record as pervasively altered.
Here, we demonstrate that cherts are a robust archive of diagenetic temperatures, despite metamorphism and exposure to meteoric fluids, and show that the timing and temperature of quartz precipitation and thus δ18Ochert are determined by the kinetics of silica diagenesis. A diagenetic model shows that δ18Ochert is influenced by heat flow through the sediment column. Heat flow has decreased over time as planetary heat is dissipated, and reasonable Archean-modern heat flow changes account for ~5‰ of the increase in δ18Ochert, obviating the need for extreme TSW or δ18Osw reconstructions. The seawater oxygen isotope budget is also influenced by solid Earth cooling, with a recent reconstruction placing Archean δ18OSW 5 to 10‰ lower than today. Together, this provides an internally consistent view of the δ18Ochert record as driven by solid Earth cooling over billion-year timescales that is compatible with Precambrian glaciations and biological.
Ratiometric green–red fluorescent nanosensors for fluorometrically monitoring pH in the acidic range were designed from 80 nm-sized polystyrene (PS) and silica (SiO2) nanoparticles (NPs), red emissive reference dyes, and a green emissive naphthalimide pH probe, analytically and spectroscopically characterized, and compared regarding their sensing performance in aqueous dispersion and in cellular uptake studies. Preparation of these optical probes, which are excitable by 405 nm laser or LED light sources, involved the encapsulation of the pH-inert red-fuorescent dye Nile Red (NR) in the core of self-made carboxylated PSNPs by a simple swelling procedure and the fabrication of rhodamine B (RhB)-stained SiO2-NPs from a silane derivative of pH-insensitive RhB. Subsequently, the custom-made naphthalimide pH probe, that utilizes a protonation-controlled photoinduced electron transfer process, was covalently attached to the carboxylic acid groups at the surface of both types of NPs. Fluorescence microscopy studies with the molecular and nanoscale optical probes and A549 lung cancer cells confirmed the cellular uptake of all probes and their penetration into acidic cell compartments, i.e., the lysosomes, indicated by the switching ON of the green naphthalimide fluorescence. This underlines their suitability for intracellular pH sensing, with the SiO2-based nanosensor revealing the best performance regarding uptake speed and stability.
This is a remote presentation I gave at the 2022 Small-angle Scattering conference in Campinas, Brazil. The video has been obtained from the conference organisers with their explicit permission for use on YouTube. I've tried to spruce up the audio from the remote recording the best I could.
The conference abstract for this talk was:
"How much do we, the small-angle scatterers, influence the results of an investigation? What uncertainty do we add by our human diversity in thoughts and approaches, and is this significant compared to the uncertainty from the instrumental measurement factors?
After our previous Round Robin on data collection, we know that many laboratories can collect reasonably consistent small-angle scattering data on easy samples[1]. To investigate the next, human component, we compiled four existing datasets from globular (roughly spherical) scatterers, each exhibiting a common complication, and asked the participants to apply their usual methods and toolset to the quantification of the results (https://lookingatnothing.com/index.ph....
Accompanying the datasets was a modicum of accompanying information to help with the interpretation of the data, similar to what we normally receive from our collaborators. More than 30 participants reported back with volume fractions, mean sizes and size distribution widths of the particle populations in the samples, as well as information on their self-assessed level of experience and years in the field.
While the Round Robin is still underway (until the 25th of April, 2022), the initial results already show significant spread in the results. Some of these are due to the variety in interpretation of the meaning of the requested parameters, as well as simple human errors, both of which are easy to correct for. Nevertheless, even after correcting for these differences in understanding, a significant spread remains. This highlights an urgent challenge to our community: how can we better help ourselves and our colleagues obtain more reliable results, how could we take the human factor out of the equation, so to speak?
In this talk, we will introduce the four datasets, their origins and challenges. Hot off the press, we will summarize the anonymized, quantified results of the Data Analysis Round Robin. (Incidentally, we will also see if a correlation exists between experience and proximity of the result to the median). Lastly, potential avenues for improving our field will be offered based on the findings, ranging from low-effort yet somehow controversial improvements, to high-effort foundational considerations."
Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies.
One-pot covalent functionalization of 2D black phosphorus by anionic ring opening polymerization
(2022)
In this work, a one-pot approach for the covalent functionalization of few-layer black phosphorus (BP) by anionic ring opening polymerization of glycidol to obtain multifunctional BP-polyglycerol (BP-PG) with high amphiphilicity for near-infrared-responsive drug delivery and biocompatibility is reported. Straightforward synthesis in combination with exceptional biological and physicochemical properties designates functionalized BP-PG as a promising candidate for a broad range of biomedical applications.
X-ray scattering and sorption data associated with the publication "Antiaromatic Covalent Organic Frameworks Based on Dibenzopentalenes". X-ray scattering data is provided for COF and POP materials, including data from stability tests, as three-column ascii files with columns q (nm-1), I (m-1) and uncertainty on I, as well as being provided in 2θ.
As virus outbreaks continue to pose a challenge, a nonspecific viral inhibitor can provide significant benefits, especially against respiratory viruses. Polyglycerol sulfates recently emerge as promising agents that mediate interactions between cells and viruses through electrostatics, leading to virus inhibition.
Similarly, hydrophobic C60 fullerene can prevent virus infection via interactions with hydrophobic cavities of surface proteins. Here, two strategies are combined to inhibit infection of SARS-CoV-2 variants in vitro. Effective inhibitory concentrations in the millimolar range highlight the significance of bare fullerene’s hydrophobic moiety and electrostatic interactions of polysulfates with surface proteins of SARS-CoV-2. Furthermore, microscale thermophoresis measurements support that fullerene linear polyglycerol sulfates interact with the SARS-CoV-2 virus via its spike protein, and highlight importance of electrostatic interactions within it. All-atom molecular dynamics simulations reveal that the fullerene binding site is situated close to the receptor binding domain, within 4 nm of polyglycerol sulfate binding sites, feasibly allowing both portions of the material to interact simultaneously.
Reliable and straightforward characterization and analysis of carbon-based nanomaterials on the atomic level is essential to exploring their potential for application. Here we use a combination of highly surface sensitive x-ray photoelectron (XP) spectroscopy and near edge x-ray absorption fine structure spectroscopy (NEXAFS) to study and quantify the covalent functionalization of nanographene and single-walled carbon nanotubes with nitrene [2 + 1]-cycloaddition. With this comprehensive analytical approach, we demonstrate that the π-conjugated system of functionalized carbon-based nanomaterials is preserved according to NEXAFS analysis, which is challenging to prove with XP spectroscopy investigation alone. Using this combination of analytical approaches, we show significant similarities after functionalization for various carbon-based nanomaterials. Both analytical methods are strongly suited to study possible post-modification reactions of functionalized carbon-based nanomaterials.
The Federal Institute for Materials Research and Testing (BAM) organised an interlaboratory comparison (ILC) for the characterisation of 87Sr/86Sr isotope ratios in limestone (IAG/CGL ML-3) and Penrhyn slate (IAG OU-6) reference materials by applying the conventional method for 87Sr/86Sr isotope ratios. Samples were sent to thirteen analytical laboratories . Since both samples are powdered, rock materials, dissolution of the sample and Sr isolation via ion exchange chromatography were mandatory. This was done using acid, microwave/acid, bomb/acid digestion or borate fusion and subsequent isolation of Sr by means of commercially available ion exchange resins. In this study, we present and discuss the potential effects that differences between laboratories, and between two instrumental measurement techniques (i.e., MC-ICP-MS and MC-TIMS), may have upon the dispersion of measurement results of the 87Sr/86Sr isotope ratio in the two aforementioned reference materials. We used a statistical mixed effects model to assess the potential effects of both the laboratory and the measurement technique. Consensus values for both materials and associated standard uncertainties {(IAG/CGL ML-3 (0.708245±0.000004) mol/mol; IAG OU-6 (0.729769±0.000008) mol/mol} were estimated by fitting a linear, Gaussian mixed effects model (Pinheiro and Bates 2000) using the R function “lmer” defined in package “lme4”. The statistical results showed that there is no significant effect attributable to differences between instrumental techniques when both materials are considered together, or separately. The p-value of the test of significance of the measurement technique effect is greater than 0.54. For both materials there were statistically significant effects attributable to differences between laboratories when the measurement results for both materials were considered together and separately. This effect is less than 0.00004 in absolute value. However, for neither material did consideration or disregard for such differences induce significant changes in the estimate of the consensus value for the 87Sr/86Sr isotope ratio. Therefore, the effects attributable to differences between instrumental techniques or between laboratories can safely be disregarded when computing the best estimate for the true value of 87Sr/86Sr isotope ratio in these materials, by the community of expert laboratories represented in this study.
Constant interactions between tumor cells and the extracellular matrix (ECM) influence the progression of prostate cancer (PCa). One of the key components of the ECM are collagen fibers, since they are responsible for the tissue stiffness, growth, adhesion, proliferation, migration, invasion/metastasis, cell signaling, and immune recruitment of tumor cells. To explore this molecular marker in the content of PCa, we investigated two different tumor volumes (500 mm3 and 1000 mm3) of a xenograft mouse model of PCa with molecular magnetic resonance imaging (MRI) using a collagen-specific probe. For in vivo MRI evaluation, T1-weighted sequences before and after probe administration were analyzed. No significant signal difference between the two tumor volumes could be found. However, we detected a significant difference between the signal intensity of the peripheral tumor area and the central area of the tumor, at both 500 mm3 (p < 0.01, n = 16) and at 1000 mm3 (p < 0.01, n = 16). The results of our histologic analyses confirmed the in vivo studies: There was no significant difference in the amount of collagen between the two tumor volumes (p > 0.05), but within the tumor, higher collagen expression was observed in the peripheral area compared with the central area of the tumor. Laser ablation with inductively coupled plasma mass spectrometry further confirmed these results. The 1000 mm3 tumors contained 2.8 +- 1.0% collagen and the 500 mm3 tumors contained 3.2 +- 1.2% (n = 16). There was a strong correlation between the in vivo MRI data and the ex vivo histological data (y = 0.068x + 1.1; R2 = 0.74) (n = 16). The results of elemental analysis by inductively coupled plasma mass spectrometry supported the MRI data (y = 3.82x + 0.56; R2 = 0.79; n = 7). MRI with the collagen-specific probe in PCa enables differentiation between different tumor areas. This may help to differentiate tumor from healthy tissue, potentially identifying tumor areas with a specific tumor biology.
In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other.
The generation of ozone and nitrogen oxides by laser-induced dielectric breakdown (LIDB) in mixtures of air with noble gases Ar, He, Kr, and Xe is investigated using OES and IR spectroscopy, mass spectrometry, and absorption spectrophotometry. It is shown that the formation of NO and NO2 noticeably depends on the type of inert gas; the more complex electronic configuration and the lower ionization potential of the inert gas led to increased production of NO and NO2. The formation of ozone occurs mainly due to the photolytic reaction outside the gas discharge zone. Equilibrium thermodynamic analysis showed that the formation of NO in mixtures of air with inert gases does not depend on the choice of an inert gas, while the equilibrium concentration of the NO+ ion decreases with increasing complexity of the electronic configuration of an inert gas.
Nanoparticles (NPs) have become important materials for a variety of chemical technologies, including catalysis. One of the main challenges is the reduction of green house gases, such as CO2. One opportunity besides the capturing is the conversion to synthesis gas via the reverse water-gas shift reaction.
A facile and efficient method is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core-shell NPs. The diameter of the NPs can be tuned in a range from 6 nm to 30 nm and the Ni:Cu ratio from 30:1 to 1:1. The NPs are structurally characterized with combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray photoelectron spectroscopy, and X-ray absorption fine structure. Using these analytical methods, a core-shell-shell structure their chemical composition is elucidated. A depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core-shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction).
Sediments and soils can act as sinks of species of inorganic mercury (Hg2+), while they are simultaneously sources of organic species, such as monomethylmercury (MMHg). Although the fraction of MMHg in total Hg of sediments is suggested to be only 0.1–1%, MMHg poses a threat for humans and wildlife due to its toxic properties, high bioaccumulation potential and the ability to pass the blood-brain barrier. One example of a highly Hg contaminated waterbody is the Finow Canal, the oldest artificial waterway still in operation in Germany. Here, Hg mass fractions of up to 100 µg/g were found in the sediment in previous studies. These are suggested to be associated with a chemical plant producing mercury-based seed dressings. Despite this high mass fraction of Hg, no Hg speciation studies have been conducted there up to now.
In this study, Hg speciation in sediments of Finow Canal at locations before and after the known polluted site was conducted using species-specific isotope dilution (SSID) GC-ICP-ToF-MS. Mass fractions of up to 0.41 µg/g MMHg were determined. In addition, waterbodies around the initially polluted site were investigated and elevated concentrations were also determined around 14 km downstream. For MMHg analysis, the performance of ICP-ToF-MS for SSID GC/ICP-MS was compared with ICP-Q-MS and ICP-SF-MS. Here, isotope ratio precision was similar between the tested instruments. However, the (quasi-) simultaneous detection of the whole mass spectrum will probably offer a much higher precision of ICP-ToF-MS, when more than one isotope system is used.
These results are the first evidence of the occurrence of MMHg in this region and show the need for further investigations of the whole regional ecosystem, as well as the consideration of possible measures of remediation. SSID GC-ICP-(ToF)-MS is a suitable tool for investigating species-specific (multi) isotope systems for environmental monitoring.
Simulates X-ray and Neutron scattering patterns from arbitrary shapes defined by STL files.
Features:
- Uses multithreading to compute a number of independent solutions, then uses the variance of the results to estimate an uncertainty on the output.
- Can be launched from the command line using an excel sheet to define settings, or from a jupyter notebook.
- Outputs scattering patterns in absolute units if the contrast is set.
- A Gaussian size distribution is available, where the relative scaling of objects for each repetion can be varied. Recommended to be used with limited width (max. 10%) to avoid artefacts.
- Writes results with settings to an archival HDF5 file.
Application examples:
This software has been used in several studies to date. For example, it has been used here to simulate a model scattering pattern for a cuboid shape, which was then fed forward into the McSAS3 analysis program for analyzing scattering patterns of polydisperse cuboids. A second use is here, where it was used for the modeling of flattened helices. In this paper, scattering pattern features could be matched with particular morphological changes in the structure. Lastly, this paper has an example where it was used to validate the analytical analysis model, and explore the realistic limits of application of the analytical model.
Since its discovery, graphene has got growing attention in the industrial and application research due to its unique properties . However, graphene has not been yet implemented into the industrial market, in particularly due to the difficulty of properly characterizing this challenging material. As most of other nanomaterials, graphene’s properties are closely linked to its chemical and structural properties, such as number of layers, flake thickness, degree of functionalisation and C/O ratio. For the commercialization, suitable procedures for the measurement and characterization of the ultrathin flakes, of lateral dimensions in the range from µm to tens of µm, are essential.Surface chemical methods, especially XPS, have an outstanding role of providing chemical information on the composition. Thereby, one well-known problem for surface analytical methods is the influence of contamination on the composition as in the case of adventitious carbon. The differentiation between carbon originated from the contamination or from the graphene sample itself is often not obvious, which can lead to altered results in the determination of the composition. To overcome this problem, Hard Energy X-ray Photoelectron Spectroscopy (HAXPES) offers new possibilities due to its higher information depth. Therefore, XPS measurement obtained with Al Kα radiation (E = 1486. 6 eV) were compared with analyses performed with a Cr Kα (E = 5414. 8 eV) excitation on functionalized graphene samples. Differences are discussed in terms of potential carbon contamination, but also of oxygen on the composition of the samples. Measurements are performed on O-, N- and F-functionalized graphene. Different preparation procedures (powder, pellet, drop cast from liquid suspension) will be also discussed, correlation of the results with the flakes morphology as well as their validation with other independent methods are in progress.
This work explores the feasibility of producing bead-on-plate welds of a CrCoNi medium entropy alloy and a CrMnFeCoNi high entropy alloy using electron beam welding. The alloys were welded in two states: one in an as-cold-rolled condition and the other in an annealed condition. In addition, the materials are welded with two different parameters. The FCC microstructure of the welds is investigated using scanning electron microscopy assisted by energy-dispersive X-ray spectroscopy and electron-backscattered diffraction. The impact of the weld on the microstructure is discussed. The heat-affected zone is negligible for the annealed condition of both medium and high entropy alloys since there is no driving force for recrystallisation and the exposure time to high temperature is insufficient for grain coarsening. The texture formed in the fusion zone is also discussed and compared to the texture in the base metal and the heat-affected zone. Although the grain growth along the (100) crystallographic direction is preferential in all cases, the crystallographic texture type differs from each weld. Higher hardness values are measured in the medium entropy alloy’s base metal and fusion zone than in the high entropy alloy.
This dataset contains the processed and analysed small-angle X-ray scattering data associated with all samples from the publications "Bio-SAXS of Single-Stranded DNA-Binding Proteins: Radiation Protection by the Compatible Solute Ectoine" (https://doi.org/10.1039/D2CP05053F).
Files associated with McSAS3 analyses are included, alongside the relevant SAXS data, with datasets labelled in accordance to the protein (G5P), its concentration (1, 2 or 4 mg/mL), and if Ectoine is present (Ect) or absent (Pure). PEPSIsaxs simulations of the GVP monomer (PDB structure: 1GV5 ) and dimer are also included.
TOPAS-bioSAXS-dosimetry extension for TOPAS-nBio based particle scattering simulations can be obtained from https://github.com/MarcBHahn/TOPAS-bioSAXS-dosimetry which is further described in https://doi.org/10.26272/opus4-55751.
This work was funded by the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) under grant number 442240902 (HA 8528/2-1 and SE 2999/2-1). We acknowledge Diamond Light Source for time on Beamline B21 under Proposal SM29806. This work has been supported by iNEXT-Discovery, grant number 871037, funded by the Horizon 2020 program of the European Commission.
Small-angle scattering data analysis round robin - Anonymized results, figures and Jupyter notebook
(2023)
The intent of this round robin was to find out how comparable results from different researchers are, who analyse exactly the same processed, corrected dataset.
This zip file contains the anonymized results and the jupyter notebook used to do the data processing, analysis and visualisation. Additionally, TEM images of the samples are included.
These are four datasets that were made available to the participants of the Small-angle Scattering data analysis round robin. The intent was to find out how comparable results from different researchers are, who analyse exactly the same processed, corrected dataset.
In this repository, there are:
1) a PDF document with more details for the study,
2) the datasets for people to try and fit,
3) an Excel spreadsheet to document the results.
Datasets 1 and 2 were modified from: Deumer, Jerome, & Gollwitzer, Christian. (2022). npSize_SAXS_data_PTB (Version 5) [Data set]. Zenodo. https://doi.org/10.5281/zenodo.5886834
Datasets 3 and 4 were collected in-house on the MOUSE instrument.
This study investigates the non-destructive detection of delaminations in concrete plates using non-contact laser ablation, instead of the conventional hammer excitation, as part of the impact echo method. We performed tests on five concrete specimens of different sizes, two of which contained artificial delaminations. A range of steel ball hammers was used as reference impulse sources, the responses of which were compared with wave excitation generated by a 7 ns pulsed 1064 nm Nd:YAG laser with 150 mJ pulse energy. Signals were recorded by surface-mounted accelerometers and two contactless methods: microphones and a laser Doppler vibrometer. The laser generates frequencies across a broad range of frequencies (0 to 150 kHz) but with much less energy than the hammers' narrower frequency spectra; the laser pulse energy transferred into the specimen is 0.07 mJ, corresponding to about 0.5 ‰ of the impulse source energy. Because of this, the thick intact plates' characteristic thickness stretch resonance frequency can be reliably detected by the hammer excitations but not when using laser excitation. However, the laser can excite low-frequency flexural vibration modes over a shallow delamination at 3 cm depth. The low-frequency flexural vibration results are verified by numerical natural frequency analysis.
McSAS3
(2023)
McSAS3 is a refactored version of the original McSAS (see DOI 10.1107/S1600576715007347). This software fits scattering patterns to obtain size distributions without assumptions on the size distribution form. The refactored version has some neat features:
- Multiprocessing is included, spread out over as many cores as number of repetitions!
- Full state of the optimization is stored in an organized HDF5 state file.
- Histogramming is separate from optimization and a result can be re-histogrammed as many times as desired.
- SasModels allow a wide range of models to be used
- If SasModels does not work (e.g. because of gcc compiler issues on Windows or Mac), an internal sphere model is supplied
- Simulated data of the scattering of a special shape can also be used as a McSAS fitting model. Your models are infinite!
- 2D fitting also works.
The need for quality assessment of anthropogenic impact on environmental pollution is increasing due to discharge from various industries, the use of chemicals in agriculture and the consumption of fossil fuels. Diminishing resources such as natural waters used for the cultivation of agricultural products, plant and animal habitats are under severe pollution pressure and are at constant risk. Several parameters, such as Pb, Cd, Ni, Hg were listed by Water Framework Directive in Directive(2008/105/EC) in the priority substances. Cadmium and Hg were identified as priority hazardous substances whereas As is an important contaminant for its potential toxicological and carcinogenic effects. An inter-comparison study is organised in EURAMET TC-MC in order to demonstrate the capability participants for measuring five elements in river water. The participants carried out measurements for analytes: Pb, Cd, Ni and As as mandatory elements, and Se as an optional one. Participants were asked to perform the measurements with respect to the protocol provided. 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).
Soft polymers such as the investigated polyurethane, characterized by low Young’s moduli and prone to high shear deflection, are frequently applied in pneumatic cylinders. Their performance and lifetime without external lubrication are highly determined by the friction between seal and shaft and the wear rate. FEM simulation has established itself as a tool in seal design processes but requires input values for friction and wear depending on material, load, and velocity. This paper presents a tribological test configuration for long stroke, reciprocating movement, allowing the generation of data which meet the requirements of input parameters for FEM simulations without the geometrical influences of specific seal profiles. A numerical parameter study, performed with an FEM model, revealed the most eligible sample geometry as a flat, disc-shaped sample of the polymer glued on a stiff sample holder. At the same time, the study illustrates that the sensitivity of the contact pressure distribution to Poisson’s ratio and CoF can be minimized by the developed and verified setup. It ensures robust, reliable, and repeatable experimental results with uniform contact pressures and constant contact areas to be used in databases and FEM simulations of seals, enabling upscaling from generically shaped samples to complex seal profiles.
Technical drawings and documents for building a compact, heated, vacuum compatible flow-through sample holder. This holder is in use at the BAM MOUSE instrument as well as at the I22 beamline at the Diamond Light Source (see references for instrument details).
This holder has several features:
- The holder can be used in vacuum environments as well as in atmosphere
- It has two G 1/4" UNF fittings to attach HPLC tubing for (optionally) flowing a medium through the sample cell
- There are two additional (unflowed) sample positions for backgrounds and calibrants, held at the same temperature
- The low-mass design coupled with a 250W heating element can achieve heating rates of 1 degree C per second, when coupled (for example) with an Omron E5CC PID controller.
- The sample holder insert can be made from various materials depending on the application. Sealing the sample from the vacuum can be achieved using kapton, teflon or Magic tape, depending on the temperature requirements. The inlet and outlet holes will need to be punctured with a needle to enable flow.
- Large exit cones ensure a clear exit angle of at least 45 degrees two theta.
- It has been tested with temperatures up to 400 degrees C.
- Compression area has been raised and polished to ensure a good vacuum seal.
OpenSCAD, STL and technical drawings for the solid sample rack designed primarily for use with The MOUSE instruments.
This solid sample rack can be used in conjunction with:
- Laser-cut sample holder (10.5281/zenodo.7499437)
- Modular sample holder (10.5281/zenodo.7499416)
- Capillary flow-cell for liquid samples (10.5281/zenodo.7499421)
PDF file for the laser-cut sample holder designed primarily for use with The MOUSE instruments.
This sample holder can be used in conjunction with:
- Solid sample rack/plate (10.5281/zenodo.7499424)
- Modular sample holder (10.5281/zenodo.7499416)
- Capillary flow-cell for liquid samples (10.5281/zenodo.7499421)
OpenSCAD, STL and technical drawings for the capillary flow-through cell designed primarily for use with The MOUSE instruments.
This flow-through cell can be used in conjunction with:
- Modular sample holder (10.5281/zenodo.7499416)
- Solid sample rack/plate (10.5281/zenodo.7499424)
- Laser-cut sample holder (10.5281/zenodo.7499437)
OpenSCAD, STL and technical drawings for the Modular sample holder designed primarily for use with The MOUSE instruments.
This modular sample holder can be used in conjunction with the following:
- Capillary flow-cell for liquid samples (10.5281/zenodo.7499421)
- Solid sample rack/plate (10.5281/zenodo.7499424)
- Laser-cut sample holder (10.5281/zenodo.7499437)
X-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved in situ (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) setup allows us to increase the time resolution over existing fluorescence measurements from ∼15 min to 2 s for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis and (ii) the synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to using TRIS-DXAS for following conventional ball milling reactions. We expect that our TRIS-DXAS approach will become an essential part of the mechanochemical tool box.
In mass spectrometry based proteomics, protein homology leads to
many shared peptides within and between species. This complicates
taxonomic inference. inference. We introduce PepGM, a graphical model for taxonomic profiling of viral proteomes and metaproteomic datasets.
Using the graphical model, our approach computes statistically sound
scores for taxa based on peptide scores from a previous database
search, eliminating the need for commonly used heuristics.
In mass spectrometry based proteomics, protein homology leads to
many shared peptides within and between species. This complicates
taxonomic inference. inference. We introduce PepGM, a graphical model for taxonomic profiling of viral proteomes and metaproteomic datasets.
Using the graphical model, our approach computes statistically sound
scores for taxa based on peptide scores from a previous database
search, eliminating the need for commonly used heuristics.
In mass spectrometry based proteomics, protein homology leads to
many shared peptides within and between species. This complicates
taxonomic inference. inference. We introduce PepGM, a graphical model for taxonomic profiling of viral proteomes and metaproteomic datasets.
Using the graphical model, our approach computes statistically sound
scores for taxa based on peptide scores from a previous database
search, eliminating the need for commonly used heuristics.
In mass spectrometry based proteomics, protein homology leads to
many shared peptides within and between species. This complicates
taxonomic inference. inference. We introduce PepGM, a graphical model for taxonomic profiling of viral proteomes and metaproteomic datasets.
Using the graphical model, our approach computes statistically sound
scores for taxa based on peptide scores from a previous database
search, eliminating the need for commonly used heuristics. heuristics.
In mass spectrometry based proteomics, protein homology leads to
many shared peptides within and between species. This complicates
taxonomic inference. inference. We introduce PepGM, a graphical model for taxonomic profiling of viral proteomes and metaproteomic datasets.
Using the graphical model, our approach computes statistically sound
scores for taxa based on peptide scores from a previous database
search, eliminating the need for commonly used heuristics. heuristics.
Probability based taxonomic profiling of viral and microbiome samples using PepGM and Unipept
(2022)
In mass spectrometry based proteomics, protein homology leads to many shared peptides within and between species. This complicates
taxonomic inference in samples of unknown taxonomic origin. PepGM uses a graphical model for taxonomic profiling of viral proteomes and
metaproteomic datasets providing taxonomic confidence scores. To build the graphical model, a list of potentially present taxa needs to be
inferred. To this end, we integrate Unipept, which enables the fast querying of potentially present taxa. Together, they allow for taxonomic
inference with statistically sound confidence scores.