Improved performance of neutron activation analysis laboratories by feedback workshops following interlaboratory comparison rounds.

The International Atomic Energy Agency (IAEA) implemented an innovative project for assisting neutron activation analysis laboratories in improving the validity of their results by feedback workshops for discussion of results from participation in interlaboratory comparisons rounds in 2010. The participants learned during these meetings to identify the most probable sources of errors in their analytical procedures and how to implement corrective actions to prevent reoccurrence. The outcome of successive rounds between 2010 and 2018 is discussed and experiences during the feedback workshops are given. The quantitative evaluation of the results shows an overall improvement in satisfactory performance. Moreover, there is a clear indication that improvements are consolidated in most laboratories but also stimulate laboratories to develop to a higher level of excellence. Regional differences in performance are also analysed.

Observation of a martensitic structural distortion in V, Nb, and Ta.

Thermal-expansion measurements of the Group 5 elements V, Nb, and Ta reveal a structural distortion below 300 K. Data for single-crystalline Nb and Ta display anisotropic thermal expansion, martensitic in character, that is inconsistent with cubic crystal structures at low temperature. Published results on V show similar behavior. Interstitial impurities suppress the transition.

CdSe spherical quantum dots stabilised by thiomalic acid: biphasic wet synthesis and characterisation.

CdSe quantum dots stabilised by thiomalic acid have been synthesised by an aqueous biphasic ligand exchange reaction in air. The materials are completely water-soluble and were found to be stable over a long time. X-ray diffraction and transmission electron microscopy reveal the formation of CdSe nanocrystals with cubic structure (a=0.6077 nm; spatial group: F-43m). The average particle size is about 5 nm. Energy dispersive X-ray analysis shows that the nanocrystals are nonstoichiometric, with a Cd/Se ratio varying between 60/40 and 70/30, and indicates the presence of Cd(2+) ions at the nanocrystal surface. Diffuse reflectance infrared Fourier transform measurements suggest that thiomalic acid chelates CdSe through the thiol group and one carboxylic function, while the second COOH group is semi-free. A complex-like structure is proposed, in which thiomalic acid forms a five-membered chelate ring with the Cd(2+) ions present on the nanocrystal surface. Chelate effect accounts for the easiness of ligand exchange and is expected to additionally stabilise the nanosystem.

Polycrystalline gamma-plutonium's elastic moduli versus temperature.

Resonant ultrasound spectroscopy was used to measure the elastic properties of pure polycrystalline (239)Pu in the gamma-phase. Shear and longitudinal elastic moduli were measured simultaneously and the bulk modulus was computed from them. A smooth, linear, and large decrease in all elastic moduli with increasing temperature was observed. The Poisson ratio was calculated and an increase from 0.242 at 519 K to 0.252 at 571 K was found. These measurements on extremely well-characterized pure Pu are in agreement with other reported results where overlap occurs. We calculated an approximate Debye temperature Theta(D)=144 K. Determined from the temperature variation in the bulk modulus, gamma-Pu shows the same Gruneisen parameter as copper.

Quantum limit transport and destruction of the Weyl nodes in TaAs.

Weyl fermions are a recently discovered ingredient for correlated states of electronic matter. A key difficulty has been that real materials also contain non-Weyl quasiparticles, and disentangling the experimental signatures has proven challenging. Here we use magnetic fields up to 95 T to drive the Weyl semimetal TaAs far into its quantum limit, where only the purely chiral 0th Landau levels of the Weyl fermions are occupied. We find the electrical resistivity to be nearly independent of magnetic field up to 50 T: unusual for conventional metals but consistent with the chiral anomaly for Weyl fermions. Above 50 T we observe a two-order-of-magnitude increase in resistivity, indicating that a gap opens in the chiral Landau levels. Above 80 T we observe strong ultrasonic attenuation below 2 K, suggesting a mesoscopically textured state of matter. These results point the way to inducing new correlated states of matter in the quantum limit of Weyl semimetals.

Alpha-plutonium's polycrystalline elastic moduli over its full temperature range.

alpha-plutonium's volume-corrected polycrystal elastic moduli were measured between 18 K and the upper limit of its occurrence, near 400 K. The two independent moduli for a polycrystal-bulk and shear-behave smoothly, indicating no phase transition. Both moduli show the same 50% increase on cooling, an order of magnitude larger than in other metals. The Debye temperature obtained from low-temperature elastic moduli, 207 K, significantly exceeds most previous estimates. The Gruneisen parameter gamma=5.3, obtained from the temperature dependence of the bulk modulus, is intermediate among previous estimates using other approaches, alpha-plutonium's Poisson ratio nu is low: 0.18, nearly temperature independent, and its small decrease on warming opposes usual behavior. The high gamma, large but equal bulk modulus and shear modulus fractional stiffening on cooling, and near-temperature-invariant nu are attributed to a single mechanism: 5-f electron localization-delocalization.

Assessment of PM2.5 sources and their corresponding level of uncertainty in a coastal urban area using EPA PMF 5.0 enhanced diagnostics.

Datasets that include only the PM elemental composition and no other important constituents such as ions and OC, should be treated carefully when used for source apportionment. This work is demonstrating how a source apportionment study utilizing PMF 5.0 enhanced diagnostic tools can achieve an improved solution with documented levels of uncertainty for such a dataset. The uncertainty of the solution is rarely reported in source apportionment studies or it is reported partially. Reporting the uncertainty of the solution is very important especially in the case of small datasets. PM2.5 samples collected in Patras during the year 2011 were used. The concentrations of 22 elements (Z=11-33) were determined using PIXE. Source apportionment analysis revealed that PM2.5 emission sources were biomass burning (11%), sea salt (8%), shipping emissions (10%), vehicle emissions (33%), mineral dust (2%) and secondary sulfates (33%) while unaccounted mass was 3%. Although Patras city center is located in a very close proximity to the city's harbor, the contribution of shipping originating emissions was never before quantified. As rotational stability is hard to be achieved when a small dataset is used the rotational stability of the solution was thoroughly evaluated. A number of constraints were applied to the solution in order to reduce rotational ambiguity.

Assessment of measurement result uncertainty in determination of (210)Pb with the focus on matrix composition effect in gamma-ray spectrometry.

Reference materials were used to assess measurement result uncertainty in determination of (210)Pb by gamma-ray spectrometry, liquid scintillation counting, or indirectly by alpha-particle spectrometry, using its daughter (210)Po in radioactive equilibrium. Combined standard uncertainties of (210)Pb massic activities obtained by liquid scintillation counting are in the range 2-12%, depending on matrices and massic activity values. They are in the range 1-3% for the measurement of its daughter (210)Po using alpha-particle spectrometry. Three approaches (direct computation of counting efficiency and efficiency transfer approaches based on the computation and, respectively, experimental determination of the efficiency transfer factors) were applied for the evaluation of (210)Pb using gamma-ray spectrometry. Combined standard uncertainties of gamma-ray spectrometry results were found in the range 2-17%. The effect of matrix composition on self-attenuation was investigated and a detailed assessment of uncertainty components was performed.

QED v 1.0: a software package for quantitative electron diffraction data treatment.

A new software package for quantitative electron diffraction data treatment of unknown structures is described. No "a priori" information is required by the package which is able to perform in successive steps the 2-D indexing of digitised diffraction patterns, the extraction of the intensity of the collected reflections and the 3-D indexing of all recorded patterns, giving as results the lattice parameters of the investigated structure and a series of data files (one for each diffraction pattern) containing the measured intensities and the relative e.s.d.s of the 3-D indexed reflections. The software package is mainly conceived for the treatment of diffraction patterns taken with a Gatan CCD Slow-Scan Camera, but it can also deal with generic digitised plates. The program is designed to extract intensity data suitable for structure solution techniques in electron crystallography. The integration routine is optimised for a correct background evaluation, a necessary condition to deal with weak spots of irregular shape and an intensity just above the background.

Comparison of spatial resolutions obtained with different signal components in scanning electron microscopy.

Comparative studies on the ultimate spatial resolution of the Scanning Electron Microscope, using different components of the electron signal have been performed on specimens providing compositional contrast. By operating the microscope in conventional way as well as with a specifically designed set-up we have ascertained that the delocalized components of the signal provide a spatial resolution of the order of the beam size, even if the practical use can be limited by the noise. To amplify the contribution of the delocalized components of the signal, as backscattered electrons by a bulk specimen or forward scattered electrons by a thin specimen, we used a device consisting of a plate of a material with high secondary yield placed above or below the sample. An important practical implication arises from this study. A detecting system consisting of a standard Everhart-Thornley detector coupled with a converter of backscattered or transmitted electrons represents a high performance detecting device for low voltage observations.

Spatial resolution and energy filtering of backscattered electron images in scanning electron microscopy.

Numerical simulations of energy filtering effects on backscattered electron images of semiconductor multilayers are reported. The theoretical investigation has been performed for a wide range of energies, 1-40 keV, and for beam incidence angles between 90 degrees (normal incidence) and 20 degrees. Quite a general purpose of this research concerns the investigation of the optimum energy conditions and of their implications. It will be shown that the optimum energy defines an operating context suitable to ensure a compositional contrast enhancement; i.e. a minimum threshold current and a maximum resolution, without energy filtering, independent of the beam incidence angle. This optimum energy, depending on the specimen and its details, is, however, of the order of a few keV or less for specimen details having a size of the order of few nm. When the performance of the electron gun does not allow to work at low energy it is necessary to operate at an energy higher than the optimum one, the energy filtering can produce positive effects. Yet in those circumstances there is an optimum energy loss window suitable to minimise the threshold current. It spreads from 10-30%, depending on the primary energy and size of the compositional detail, for normal incidence, to a few per cent for high incidence angles and high energy. The simulation results for these last conditions are in agreement with the well-known experimental results obtained with the low-loss methods.

An integrated approach to assess air pollution threats to cultural heritage in a semi-confined environment: the case study of Michelozzo's Courtyard in Florence (Italy).

An example of an integrated approach to assess air pollution threats to cultural heritage in a semi-confined environment is presented in this work, where the monitoring campaign carried out at the Michelozzo's Courtyard (in Palazzo Vecchio, Florence, Italy) is used as a case study. A wide research project was carried out, with the main aim of obtaining the first quantitative data on air quality and microclimate conditions inside the Courtyard, and, if possible, identifying the main causes of degradation and suggesting appropriate conservation strategies. The investigation adopted a holistic approach involving thermographic measurements on the wall paintings, microclimatic analysis, gaseous pollutant monitoring, atmospheric particles characterisation and dry deposition compositional analysis. Attention was focused on the wall painting depicting the city of Hall because of its anomalous and critical conservation conditions, which are visible at a glance, due to the contrast between a wide darker zone around the central subject of the painting and external lighter areas.