Evaluation of specimen preparation techniques for micro-PIXE localisation of elements in hyperaccumulating plants

Hybanthus floribundus subsp. floribundus, a rare Australian Ni-hyperaccumulating shrub and Pityrogramma calomelanos var. austroamericana, an Australian naturalized As-hyperaccumulating fern are promising species for use in phytoremediation of contaminated sites. Micro-proton-induced X-ray emission (μ-PIXE) spectroscopy was used to map the elemental distribution of the accumulated metal(loid)s, Ca and K in leaf or pinnule tissues of the two plant species. Samples were prepared by two contrasting specimen preparation techniques: freeze-substitution in tetrahydrofuran (THF) and freeze-drying. The specimens were analysed to compare the suitability of each technique in preserving (i) the spatial elemental distribution and (ii) the tissue structure of the specimens. Further, the μ-PIXE results were compared with concentration of elements in the bulk tissue obtained by ICP-AES analysis.In H. floribundus subsp. floribundus, μ-PIXE analysis revealed Ni, Ca and K concentrations in freeze-dried leaf tissues were at par with bulk tissue concentrations. Elemental distribution maps illustrated that Ni was preferentially localised in the adaxial epidermal tissues (1% DW) and least concentration was found in spongy mesophyll tissues (0.53% DW). Conversely, elemental distribution maps of THF freeze-substituted tissues indicated significantly lower Ni, Ca and K concentrations than freeze-dried specimens and bulk tissue concentrations. Moreover, Ni concentrations were uniform across the whole specimen and no localisation was observed.In P. calomelanos var. austroamericana freeze-dried pinnule tissues, μ-PIXE revealed statistically similar As, Ca and K concentrations as compared to bulk tissue concentrations. Elemental distribution maps showed that As localisation was relatively uniform across the whole specimen. Once again, THF freeze-substituted tissues revealed a significant loss of As compared to freeze-dried specimens and the concentrations obtained by bulk tissue analysis.The results demonstrate that freeze-drying is a suitable sample preparation technique to study elemental distribution of ions in H. floribundus and P. calomelanos plant tissues using μ-PIXE spectroscopy. Furthermore, cellular structure was preserved in samples prepared using this technique.     

In situ determination of radon concentration and total gamma radiation in Kastel Gomilica, Croatia

To determine current radiation background of the environment at the “Giricic” location in Kastel Gomilica, Croatia, in situ measurement of radon concentration (²²²Rn and ²²⁰Rn) in an open atmosphere on a ground level and at the height of 1.5 m has been made as well as total gamma radiation at the height of 1 m in an energy range of 15 keV to 2 MeV. The researched location was divided in three specific parts: (i) regulated area with the bottom ash and flying ash in the basis (“old” depot), (ii) unregulated area with waste materials, including bottom ash and flying ash, in the basis (“new” depot), (iii) uncontaminated area with no waste materials deposited on. Average radon concentration on a ground level was 213 Bq/m³ for the “old” depot, 214 Bq/m³ for the “new” depot and 59 Bq/m³ for the uncontaminated area and at the height of 1.5 m 20 Bq/m³ for the “old” depot, 34 Bq/m³ for the “new” depot and 26 Bq/m³ for the uncontaminated area. Average total gamma radiation values in selected energy range were 109.92 cps (counts per second) for the “old” depot, 357.76 cps for the “new” depot and 65.97 cps for the uncontaminated area. For selected radionuclides (²¹⁴Pb, ¹³⁷Cs, ²²⁸Ac, ^234mPa, ⁴⁰K and ²¹⁴Bi) average gamma radiation values at characteristic energies have been determined as well.     

Hyperfine interactions in the itinerant system UFeGa5

We report ⁶⁹Ga NMR measurements on the itinerant compound UFeGa₅ using a single crystal sample. Hyperfine coupling constants at both the Ga(1) and Ga(2) sites are determined for H∥a and c-axes based on Knight shift versus susceptibility plots. The T-dependence of the spin-lattice relaxation time (T₁) has been determined at both sites for H∥a and c-axes. From these quantities, the magnetic fluctuations are estimated for both axes. The complex nature of the hyperfine interactions is discussed.     

Quantitative micro-PIXE comparison of elemental distribution in Ni-hyperaccumulating and non-accumulating genotypes of Senecio coronatus

The Ni hyperaccumulator, plant species Senecio coronatus (Thunb.) Harv., Asteraceae is an example of plant adaptation mechanisms to different ecological conditions. This widespread species can inter alia be found on serpentine outcrops and the genotypes growing in serpentine soils show different ways of adaptation. The populations from two distant localities take up and translocate Ni in concentrations which are normally phytotoxic, while plants growing on a different site, in the vicinity of another hyperaccumulating species, absorb amounts which are typical for most of the plants found on serpentine soils. The NAC nuclear microprobe was used to compare the distribution of Ni and other elements in selected organs and cells with simultaneous use of PIXE and proton BackScattering (BS). Quantitative maps of stems showed large differences in concentrations and distributions of major and trace elements. In hyperaccumulating genotypes Ni is present everywhere within stem tissues, but the highest concentrations were found in the epidermis, cortex and phloem. In non-accumulating plants Ni was concentrated in the phloem. In the leaf epidermis Ni was concentrated in the cell walls for both accumulating and non-accumulating plants. These results suggest that biochemical diversity is more than morphological, because investigated genotypes belong to the same taxon.     

Semiconductor drift detectors for X- and gamma-ray spectroscopy and imaging

The semiconductor drift detectors (SDDs) show basic advantages, in terms of spectroscopic resolution and detection rate, with respect to other semiconductor detectors. These advantages are strictly related to the very low values of the output capacitance of these devices. In this paper the working principles and the performance of the SDDs are presented and the most recent devices (“droplet type” SDDs and monolithic arrays of SDDs) are introduced. The requirements of front-end electronics for the readout of the SDDs signals are then discussed and the most recent implementations (pulsed-reset preamplifiers, multi-channel ASIC readout circuits) are introduced. Some relevant applications of SDDs in the field of X-ray spectroscopy for material analysis and for nuclear physics experiments, and in the field of gamma-ray imaging, are presented as a conclusion.     

Autoionization of N (q = 1-3) Rydberg states produced in high-energy collisions with He

Energy spectra of electrons ejected through autoionization decay of high-Rydberg states in high-energy collisions of N^q+ (q = 1-3) with He have been measured with high-resolution by using zero-degree electron spectroscopy. Several series of autoionizing lines were observed, corresponding to decays from N³⁺ 1s²2p(²P)nl Rydberg states produced in N³⁺ + He collisions, from N²⁺ 1s²2s2p(³P)nl Rydberg states produced in N²⁺ + He and from N⁺ 1s²2s2p²(⁴P)nl Rydberg states produced in N⁺ + He, respectively. Angular momentum distributions for the first or second peak of three series of Coster-Kronig electron transitions for N^q+ (q = 1-3) projectiles are also discussed, where the highly excited states are formed by electron excitation.     

The interaction of antihydrogen with simple atoms and molecules

In this paper, we describe calculations that we have carried out of cross sections for rearrangement processes in very low-energy helium + antihydrogen scattering that result in or or . A significantly more accurate method from that used previously [E.A.G. Armour, S. Jonsell, Y. Liu, A.C. Todd, Nucl. Instr. and Meth. B 247 (2006) 127] is used to calculate the entrance channel wave function. Results are presented for the first two processes. Mention is made of the use of the method in calculations of low-energy e⁺H₂ scattering.     

Analysis of elemental maps from glaze to body of ancient Chinese Jun and Ru porcelain by micro-X-ray fluorescence

The reasons how the middle layer of Ru and Jun porcelain between the glaze and body came into being are still not completely understood. Here, elemental maps from the glaze to the body of pieces of ancient Chinese Ru and Jun porcelain were analyzed by micro-X-ray fluorescence. The results show the middle layer was probably formed by the chemical composition of the glaze turning into glassy states and undergoing complex physical-chemical reactions with the body. However, the middle layer of Jun porcelain was formed by the chemical composition of the glaze turning into glassy states and then infiltrating the body at high temperatures during the firing process.     

Synthesis of nanodimensional TiO2 thin films using energetic ion beam

Nanophases of TiO₂ are achieved by irradiating polycrystalline thin films of TiO₂ by 100 MeV Au ion beam at varying fluence. The surface morphology of pristine and irradiated films is studied by atomic force microscopy (AFM). Phase of the film before and after irradiation is identified by glancing angle X-ray diffraction (GAXRD). The blue shift observed in UV-vis absorption edge of the irradiated films indicates nanostructure formation. Electron spin resonance (ESR) studies are carried out to identify defects created by the irradiation. The nanocrystallisation induced by SHI irradiation in polycrystalline thin films is studied.     

Improvement on thermoelectric properties of multilayered Si1−xGex/Si by ion beam bombardment

We made n-type nano-scale thin film thermoelectric (TE) devices that consist of multiple periodic layers of Si_1−xGe_x/Si. The period is about 10 nm. The structure was modified by 5 MeV Si ion bombardment that formed a nano-scale cluster structure. In addition to the effect of confinement of the phonon transmission, formation of nanoclusters by the ionization energy of incident MeV Si ions further increases the scattering of phonons, increasing the chance of inelastic interaction of phonons, resulting in more annihilation of phonons. This limits phonon mean free path. Phonons are absorbed and dissipated along the layers rather than in the direction perpendicular to the layer interfaces, therefore cross plane thermal conductivity is reduced. The increase of the density of electronic states due to the formation of nanocluster minibands increases the cross plane Seebeck coefficient and increases the cross plane electric conductivity of the film. Eventually, the thermoelectric figure of merit of the TE film increases.     

Energy dependence of electron stopping powers in elemental solids over the 100 eV to 30 keV energy range

We analyzed the energy dependence of electron stopping powers (SPs) calculated for 41 elemental solids from experimental optical data for electron energies between 100 eV and 30 keV. Our analysis was performed with the Hill equation to represent a series of steps in plots of the slopes of Fano plots. The average root-mean-square difference between SPs from fits with an equation derived from the Hill equation and the calculated SPs was 1.0%. The new equation can provide SPs over a wide energy range for Monte Carlo simulations of electron transport with the continuous slowing-down approximation.     

Mutation effect of MeV protons on bioflocculant bacteria Bacillus cereus

A 3.2 MeV proton beam was used to irradiate bioflocculant bacteria (Bacillus cereus) to achieve mutation. The ion fluence ranged from 10¹¹ to 10¹⁴/cm². Most of the bacteria were killed when the ion fluence reached 10¹² ions/cm². The survival ratio drops in an exponential way on further increasing the ion fluence. The flocculating activity of 7 samples out of 51 showed a positive change, and a perfect mutant C7-23 with a stable high capacity of bioflocculant production was found. RAPD measurements showed that a new lane appears in this sample. The flocculating activity of the C7-23 bacteria increased by factors of 22%, 54% and 217% under pH values of 4, 7 or 10, respectively.     

Ion beam modification of strained InGaAs/InP characterized by HRXRD, PL and AFM

Highly tensile strained InGaAs/InP multi quantum wells have been grown by the LP-MOVPE technique. Such samples were subjected to irradiation with 100 MeV Au⁸⁺ ions. These were studied as a function of fluence, then the irradiated samples were annealed by rapid thermal annealing at 700 °C for 60 s in nitrogen atmosphere. We used high resolution X-ray diffraction (HRXRD), photoluminescence (PL) and atomic force microscopy (AFM) characterization techniques to study the interfacial induced changes, band gap modifications and surface morphology. Multi quantum wells were then studied before and after irradiation.     

Concentrations of U and Th in foodstuffs and radiation dose to a rural Moroccan population

Uranium (²³⁸U) and thorium (²³²Th) contents were measured in different foods widely consumed by the rural Moroccan population by using two different types of solid state nuclear track detectors (SSNTDs). The method utilized is based on determining the probabilities for α-particles emitted by the uranium and thorium series inside the studied materials to reach and be registered on the CR-39 and LR-115 type II SSNTDs and counting the resulting track densities. Total daily intakes of ²³⁸U and ²³²Th for a typical food basket were estimated to be 1.27 Bq d⁻¹ and 0.95 Bq d⁻¹, 1.55 Bq d⁻¹ and 1.18 Bq d⁻¹ and 2.01 Bq d⁻¹ and 1.52 Bq d⁻¹ for the 7-12 y, 12-17 y and adults age groups, respectively. Annual committed equivalent doses were evaluated in the human body compartments of members of the Moroccan rural population due to ²³⁸U and ²³²Th from the ingestion of the studied food materials by using the ICRP ingestion dose coefficients. Annual committed effective dose due to ²³⁸U and ²³²Th intakes were found to be 3.16 × 10⁻⁵ Sv and 10.10 × 10⁻⁵ Sv, 3.81 × 10⁻⁵ Sv and 10.80 ×  10⁻⁵ Sv and 3.32 × 10⁻⁵ Sv and 12.80 × 10⁻⁵ Sv for the 7-12 y, 12-17 y and adults age groups, respectively.     

Micro-SR-XRF and micro-PIXE studies for archaeological gold identification - The case of Carpathian (Transylvanian) gold and of Dacian bracelets

Trace-elements are more significant for provenancing archaeological metallic artifacts than the main components. For gold, the most promising elements are platinum group elements (PGE), Sn, Te, Sb, Hg and Pb. Several small fragments of natural Transylvanian gold - placer and primary - were studied by using micro-PIXE technique at the Legnaro National Laboratory AN2000 microbeam facility, Italy and at the AGLAE accelerator, C2RMF, Paris, France and by using micro synchrotron radiation X-ray fluorescence (micro-SR-XRF) at BESSY synchrotron, Berlin, Germany. The goal of the study was to identify the trace-elements, especially Sn, Sb and Te. A spectacular application to five Dacian gold bracelets authentication is presented (Sn and Sb traces).     

Ab initio approach to the effect of Fe on the diffusion in hcp Zr II: The energy barriers

Using density functional theory calculations together with the Monomer method for the search of saddle points (combined for the first time with an ab initio algorithm), we obtain the vacancy formation energies and the migration barriers for α-Zr self-diffusion and for the diffusion of interstitial impurities, including the ultra-fast diffuser Fe. Good agreement with measured diffusion coefficients is obtained, as a much lower energy barrier for the ultra-fast diffuser is found. We also suggest a possible mechanism for the increase in self-diffusion due to the Fe impurity, always present in the experimental samples.     

Swift heavy ion irradiated InGaAs/InP multi quantum wells: Band-structure, interface and surface modifications

The band-structure, interface and surface modification by swift heavy ion irradiation of In_0.55Ga_0.45As/InP multi quantum wells have been studied using photoluminescence, high resolution X-ray diffraction and atomic force microscopy. Three distinct photoluminescence peaks were observed for as-grown samples at low temperature and at room temperature the peaks merge together. Detailed analysis has been carried out to understand the origin of additional satellite peaks. A peak shift of about 23 nm was observed for irradiated samples after annealing. Highly-ordered satellite peaks were observed in X-ray scans of as-grown and Ag ion irradiated samples. In comparison, Au ion irradiated sample showed stronger interfacial degradation as seen by the diminished satellite peaks. The peak position of the irradiated samples shifted to the compressive side and was broadened in comparison with as-grown samples. The as-grown and annealed samples show smooth surfaces whereas irradiation results in nano-sized dot/island types of structures at the surface. The results are discussed in the light of complementary information provided by these techniques.     

Temperature and pressure conditions for the appropriate performance of charge and mass resolutions in balloon-borne CR-39 track detector for the heavy cosmic rays

We experimentally determined the suitable conditions of temperature and air pressure for measuring charge and mass compositions of heavy cosmic rays using CR-39 track detectors during long-duration, high-altitude balloon flights. The experiments were carried out utilizing Fe ion beams from Heavy Ion Medical Accelerator (HIMAC). Changes in the track registration sensitivity with temperature were studied at temperatures between 213 and 293 K. The charge and mass shifts around Fe ions are possibly 0.11 cu (charge unit) and 0.47 amu (atomic mass unit) at the temperature deviation between 227 and 243 K at balloon altitude. Decrease in track registration sensitivity as air pressure decreases has been observed between 13 Pa and 27 kPa. The charge and mass shifts around Fe ions are inferred to be 0.02 cu and 0.09 amu, respectively, when pressure varies between 20 and 27 kPa. During balloon flight, air pressure drops below this; therefore, care must be taken to keep the temperature and air pressure of CR-39 detectors within acceptable limits.     

Determining Pu isotopic composition and Pu content of PuBe sources by neutron coincidence technique

The paper describes a pure neutron method for determining both Pu content and Pu isotopic composition of PuBe neutron sources by neutron coincidence technique, without using gamma-spectrometry. The new procedure based on the R/T-T relationship is a developed version of the R/T-method based on R/T-M_Pu calibration curve described in [C.T. Nguyen, J. Bagi, L. Lakosi, A novel method of quantitative assay of PuBe neutron sources by neutron coincidence technique, Nucl. Instr. and Meth. B 246 (2006) 409], utilizing Pu isotopic correlations; here R, T, M_Pu are double count rate, single count rate and total Pu content, respectively. Accuracy of the method was found to be about 2-3% and 15% for ²³⁹Pu component and Pu content, respectively. Measurement time as a function of detector efficiency is treated in detail. It is shown that in a system of frame, a transuranium neutron source can be characterized by a pair of co-ordinates [R/T,  T].     

Irradiation effect on dielectric properties and electrical conductivity of Au/SiO2/n-Si (MOS) structures

The Au/SiO₂/n-Si (MOS) structures were exposed to beta-ray irradiation to a total dose of 30 kGy at room temperature. Irradiation effect on dielectric properties of MOS structures were investigated using capacitance−voltage (C−V) and conductance−voltage (G/ω−V) characteristics. The C−V and G/ω−V measurements carried out in the frequency range from 1 kHz to 10 MHz and at various radiation doses, while the dc voltage was swept from positive bias to negative bias for MOS structures. The dielectric constant (ε′), dielectric loss (ε″), loss factor (tan δ) and ac electrical conductivity (σ_ac) were calculated from the C−V and G/ω−V measurements and plotted as a function of frequency at various radiation doses. A decrease in the ε′ and ε″ were observed when the irradiation dose increased. The decrease in the ε′ and ε″ of irradiated MOS structures in magnitude is explained on the basis of Maxwell−Wagner interfacial polarization. Also, the σ_ac is found to decrease with increasing radiation dose. In addition, the values of the tan δ decrease with increasing radiation dose and give a peak. From the experimental results, it is confirmed that the peak of loss tangent is due to the interaction between majority carriers and interface states which induced by radiation.