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This study describes an interlaboratory comparison (ILC) among nine (9) laboratories to evaluate and validate the standard operation procedure (SOP) for single-particle (sp) ICP-TOFMS developed within the context of the Horizon 2020 project ACEnano. The ILC was based on the characterization of two different Pt nanoparticle (NP) suspensions in terms of particle mass, particle number concentration, and isotopic composition. The two Pt NP suspensions were measured using icpTOF instruments (TOFWERK AG, Switzerland).
Two Pt NP samples were characterized and mass equivalent spherical sizes (MESSs) of 40.4 ± 7 nm and 58.8 ± 8 nm were obtained, respectively. MESSs showed <16% relative standard deviation (RSD) among all participating labs and <4% RSD after exclusion of the two outliers. A good agreement was achieved between the different participating laboratories regarding particle mass, but the particle number concentration results were more scattered, with <53% RSD among all laboratories, which is consistent with results from previous ILC studies conducted using ICP-MS instrumentation equipped with a sequential mass spectrometer. Additionally, the capabilities of sp-ICP-TOFMS to determine masses on a particle basis are discussed with respect to the potential for particle density determination. Finally, because quasi-simultaneous multi-isotope and multielement determinations are a strength of ICP-TOFMS instrumentation, the precision and trueness of isotope ratio determinations were assessed. The average of 1000 measured particles yielded a precision of below ±1% for intensity ratios of the most abundant Pt isotopes, i.e. 194Pt and 195Pt, while the accuracy of isotope ratios with the lower abundant isotopes was limited by counting statistics.
Five distinct analytical techniques were compared for the quantification of the H2O (0·1-7·4 wt%) and D2O (up to 5·5 wt% D2O) contents in rhyolitic glasses. The hydrogen concentration in obsidians was measured using nuclear reaction analysis (NRA) and converted into H2O concentration. The bulk water content (H2O+D2O) of synthesised glasses was determined using thermal extraction in conjunction with KarlFischer titration (KFT). Unextracted H2O was measured by infrared (IR) spectroscopy after remelting the KFT products at high pressure. These well characterised glasses were subsequently used to calibrate secondary ion mass spectrometry (SIMS), infrared and evolved gas analysis (EGA). The calibrations of SIMS for H2O and D2O show a significant matrix effect at H2O and D2O concentrations larger than ~3 mol/l with the relative sensitivity factor (RSF) decreasing with bulk water content. Molar absorption coefficients for the OH stretching vibration band at 3570 cm-1 and the OD stretching vibration band at 2650 cm-1 in the infrared absorption spectra were reinvestigated. In the range 0·1-6 wt% the H2O content of glasses could be reproduced within analytical error using a constant linear molar absorption coefficient. However, it appears that the absorption coefficients for the 3570 cm-1 band as well as for the 2650 cm-1 band both decrease systematically with concentration of dissolved H2O and D2O (epsi3570=80 (±1) - 1·36(±0·23)CH2Ot and epsi2650=61·2(±1) - 2·52(± 0·30)CD2Ot). EGA allows quantification of the H2O content as well as the study of dehydration kinetics. It is shown that H2O is released under vacuum already at room temperature from glasses containing >7 wt% H2O.
The existence of microbial activity hotspots in temperate regions of Earth is driven by soil heterogeneities, especially the temporal and spatial availability of nutrients. Here we investigate whether microbial activity hotspots also exist in lithic microhabitats in one of the most arid regions of the world, the Atacama Desert in Chile. While previous studies evaluated the total DNA fraction to elucidate the microbial communities, we here for the first time use a DNA separation approach on lithic microhabitats, together with metagenomics and other analysis methods (i.e., ATP, PLFA, and metabolite analysis) to specifically gain insights on the living and potentially active microbial community. Our results show that hypolith colonized rocks are microbial hotspots in the desert environment. In contrast, our data do not support such a conclusion for gypsum crust and salt rock environments, because only limited microbial activity could be observed. The hypolith community is dominated by phototrophs, mostly Cyanobacteria and Chloroflexi, at both study sites. The gypsum crusts are dominated by methylotrophs and heterotrophic phototrophs, mostly Chloroflexi, and the salt rocks (halite nodules) by phototrophic and halotolerant endoliths, mostly Cyanobacteria and Archaea. The major environmental constraints in the organic-poor arid and hyperarid Atacama Desert are water availability and UV irradiation, allowing phototrophs and other extremophiles to play a key role in desert ecology.
The concept of a ‘plastisphere microbial community’ arose from research on aquatic plastic debris, while the effect of plastics on microbial communities in soils remains poorly understood. Therefore, we examined the inhabiting microbial communities of two plastic debris ecosystems with regard to their diversity and composition relative to plastic-free soils from the same area using 16S rRNA amplicon sequencing. Furthermore, we studied the plastic-colonizing potential of bacteria originating from both study sites as a measure of surface adhesion to UV-weathered polyethylene (PE) using high-magnification field emission scanning electron microscopy (FESEM). The high plastic content of the soils was associated with a reduced alpha diversity and a significantly different structure of the microbial communities. The presence of plastic debris in soils did not specifically enrich bacteria known to degrade plastic, as suggested by earlier studies, but rather shifted the microbial community towards highly abundant autotrophic bacteria potentially tolerant to hydrophobic environments and known to be important for biocrust formation. The bacterial inoculates from both sites formed dense biofilms on the surface and in micrometer-scale surface cracks of the UV-weathered PE chips after 100 days of in vitro incubation with visible threadlike EPS structures and cross-connections enabling surface adhesion. High-resolution FESEM imaging further indicates that the microbial colonization catalyzed some of the surface degradation of PE. In essence, this study suggests the concept of a ‘terrestrial plastisphere’ as a diverse consortium of microorganisms including autotrophs and other pioneering species paving the way for those members of the consortium that may eventually break down the plastic compounds.
The ability of industrial X-ray computed tomography (CT) to scan an object with several internal and external features at once causes increasing adoption in dimensional metrology. In order to evaluate the quality of a measurement value, the task-specific measurement uncertainty has to be determined. Currently, VDI/VDE 2630 part 2.1 gives a guideline to determine the uncertainty of CT measurements experimentally by conducting repeated measurements. This is costly and time-consuming. Thus, the aim is to determine the task-specific measurement uncertainty numerically by simulations (e. g. according to the guide to expression of uncertainty in measurement (GUM) Supplement 1). To achieve that, a digital twin is necessary. This contribution presents a simple first approach how a digital twin can be built. In order to evaluate this approach, a study comparing measurements and simulations of different real CT systems was carried out by determining the differences between the measurement results of the digital twin and of the measurement results of the real-world CT systems. The results have shown a moderate agreement between real and simulated data. To improve on this aspect, a standardized method to characterize CT systems and methods to implement CT parameters into the simulation with sufficient accuracy will be developed.
Mononuclear Fe ions ligated by nitrogen (FeNx) dispersed on nitrogen-doped carbon (Fe-N-C) serve as active centers for electrocatalytic O2 reduction and thermocatalytic aerobic oxidations. Despite their promise as replacements for precious metals in a variety of practical applications, such as fuel cells, the discovery of new Fe-N-C catalysts has relied primarily on empirical approaches. In this context, the development of quantitative structure−reactivity relationships and benchmarking of catalysts prepared by different synthetic routes and by different laboratories would be facilitated by the broader adoption of methods to quantify atomically dispersed FeNx active centers. In this study, we develop a kinetic probe reaction method that uses the aerobic oxidation of a model hydroquinone substrate to quantify
the density of FeNx centers in Fe-N-C catalysts. The kinetic method is compared with low-temperature Mössbauer spectroscopy, CO pulse chemisorption, and electrochemical reductive stripping of NO derived from NO2 − on a suite of Fe-N-C catalysts prepared by diverse routes and featuring either the exclusive presence of Fe as FeNx sites or the coexistence of aggregated Fe species in addition to FeNx. The FeNx site densities derived from the kinetic method correlate well with those obtained from CO pulse chemisorption and Mössbauer spectroscopy. The broad survey of Fe-N-C materials also reveals the presence of outliers and challenges associated with each site quantification approach. The kinetic method developed here does not require pretreatments that may alter active-site distributions or specialized equipment beyond reaction vessels and standard analytical instrumentation.
Recently, we suggested an unconventional approach (the so-called Internal-Field-Guarded-Active-Region Design “IFGARD”) for the elimination of the quantum-confined Stark effect in polar semiconductor heterostructures. The IFGARD-based suppression of the Stark redshift on the order of electronvolt and spatial charge carrier separation is independent of the specific polar semiconductor material or the related growth procedures. In this work, we demonstrate by means of micro-photoluminescence techniques the successful tuning as well as the elimination of the quantum-confined Stark effect in strongly polar [000-1] wurtzite GaN/AlN nanodiscs as evidenced by a reduction of the exciton lifetimes by up to four orders of magnitude. Furthermore, the tapered geometry of the utilized nanowires (which embed the investigated IFGARD nanodiscs) facilitates the experimental differentiation between quantum confinement and Stark emission energy shifts. Due to the IFGARD, both effects become independently adaptable.
Recently, we suggested an unconventional approach [the so-called Internal-Field-Guarded-Active-Region Design (IFGARD)] for the elimination of the crystal polarization field induced quantum confined Stark effect (QCSE) in polar semiconductor heterostructures. And in this work, we demonstrate by means of micro-photoluminescence techniques the successful tuning as well as the elimination of the QCSE in strongly polar [000-1] wurtzite GaN/AlN nanodiscs while reducing the exciton life times by more than two orders of magnitude. The IFGARD based elimination of the QCSE is independent of any specific crystal growth procedures. Furthermore, the cone-shaped geometry of the utilized nanowires (which embeds the investigated IFGARD nanodiscs) facilitates the experimental differentiation between quantum confinement- and QCSE-induced emission energy shifts. Due to the IFGARD, both effects become independently adaptable.
One of the most significant limitations for the quantum efficiency of group III-nitride based light emitters is the spatial electron-hole separation due to the quantum-confined Stark effect (QCSE). To overcome this problem, Hönig et al. [1] proposed a novel concept, the Internal-Field-Guarded-Active-Region Design (IFGARD), which suppresses the QCSE for wurtzite crystals in the [0001] direction. Here, we show how encapsulating the active region by additional guard layers results in a strong reduction of the built-in electric field in c-plane wurtzite nanostructures. Even more importantly, we demonstrate the first experimental evidence for the successful realization of an IFGARD structure based on GaN/AlN heterostructures embedded in GaN nanowires. By means of power-dependent and time-resolved µ-photoluminescence (µ-PL) we experimentally proof the validity of the unconventional IFGARD structure. We managed to tune the emission of 4-nm-thick GaN nano-discs up to 3.32 eV at low excitation powers, which is just 150 meV below the bulk GaN bandgap. Our results demonstrate an almost complete elimination of the QCSE in comparison to conventional structures which show approximately 1 eV red-shifted emission. The suppression of the QCSE results in a significant increase of the radiative exciton decay rates by orders of magnitude and demonstrates the potential of IFGARD structures for future light sources based on polar heterostructures.
[1] Hönig et al., Phys. Rev. Applied 7, 024004 (2017)
A survey is presented on some characteristic features of meteoritic (Fe,Ni)3P which is an abundant and important minor phase of most iron meteorites. This mineral (named schreibersite/rhabdite) plays a decisive role during the formation of the so-called Widmanstätten pattern. Different transmission as well as scanning electron microscopic techniques have been applied to get more precise information about the real structure of the phosphide crystals, their chemical composition and the metal distribution across the phoshide/ kamacite interface. X-ray crystal structure determinations have been performed for selected (Fe,Ni)3P - cystals from various iron meteorites (Toluca, North Chile, Watson, Orange River, Morasko, Agpalilik, Odessa, Canyon Diablo). These experiments revealed a metal ordering, i.e. for the three non-equivalent metal positions a different substitution of Fe by Ni has been found. The perfection of the brittle (Fe,Ni)3P samples differs appreciably and seems to be dependent on the thermal history of each individual meteorite. Moreover, inside Ni-rich rhabdite crystals small monocrystalline inclusions of CrN (carlsbergite) have been detected.