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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.
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.
Investigation of the orientation relationships of carlsbergite in the North Chile iron meteorite
(2005)
Subjecting a thin NiTi specimen to uniaxial tension often leads to a localized martensitic transformation: macroscopic transformation bands form and propagate through the specimen, separating it into regions of fully transformed martensite and original austenite. In the present study, the alternating current potential drop (ACPD) technique is used to analyze the change in electrical resistance of ultra-fine grained NiTi wires subjected to a broad range of thermo-mechanical load cases: (i) uniaxial tensile straining at constant temperatures (pseudoelastic deformation); (ii) cooling and heating through the transformation range at constant load (actuator load case); (iii) a combination of mechanical and thermal loading. We monitor the ACPD signals in several zones along the gauge length of specimens, and we demonstrate that a localized type of transformation is a generic feature of pseudoelastic as well as of shape memory deformation. Moreover, the ACPD signals allow to differentiate between temperature-induced martensite (formed during cooling at no or relatively small loads), stress-induced martensite, and reoriented martensite (formed under load at low temperatures).
The crystallographic orientation of carlsbergite (CrN) in the north Chile meteorite (hexahedrite) was investigated using electron backscatter diffraction and transmission electron microscopy. These studies examined the CrN crystals in the rhabdites (idiomorphic schreibersite) and in kamacite. It was found that the CrN crystals embedded in rhabdite show a number of different orientation relationships with the host crystals. These orientations can be explained based on the lattice dimensions of both coexisting crystalline materials. It was also found that both carlsbergite and kamacite are characterized by a high dislocation density (109 cm2) while rhabdite is free of dislocations. It is supposed that in spite of the deformed metallic matrix, a general connection between the orientation relation of all the phases involved exists.
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 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.