Industrial aerosol characterisation at a remote site in South Africa

South Africa is the most industrialised country in southern Africa with approximately 1.1 Tg of sulphur emitted from anthropogenic activities per annum. Complex circulation patterns and highly stable vertical atmospheric conditions promote the accumulation of pollutants below 700 hPa or 3000 m asl. A remote site in the Eastern Cape of South Africa, Ben Macdhui (30.5°S 27.9°E, 3001 m) was selected for testing the hypothesis that industrial emissions, specifically sulphate, are transported over thousands of kilometres in anticyclonic type patterns of flow and exported from the subcontinent towards the Indian Ocean at about 30°S. Time resolved particulate sampling (streaker) was conducted between June 1995 and January 1997. To characterise the industrial aerosol signal, two intensive sampling campaigns (summer and winter) were undertaken in 1996. Aerosol samples were collected by a streaker sampler and an open-faced stacked filter unit (SFU). Samples were PIXE analysed to obtain elemental concentrations. The industrial signature detected at Ben Macdhui was characterised by elevated concentration of sulphur and iron in the fine fraction and fine sulphur detected in the coarse mode. Other sources identified from the elemental data were soil (Al, Si, Ca, Mg, K, S, Mn), biomass burning (fine K) and marine (Cl, Ca, Mg, S and coarse K). These four sources accounted for approximately 70% of the total detected elemental mass. Major individual contributions came from the crustal (53%) and industrial components (21%). Air parcel trajectory analyses confirmed that peak episodes of enhanced aerosol sulphur were related to transport from the industrial Highveld region of South Africa and conversely that clean air masses originated over the southern oceans.     

Core concept of a passive-safety fast reactor “METAL-KAMADO” and reactivity coefficients

New concept of a passive-safety simple fast reactor “METAL-KAMADO” with metallic fuels is presented, which has same concept as a passive-safety thermal reactor “KAMADO”. A fuel element of the “METAL-KAMADO” consists of metallic fuel (U–10%Zr) and cooling holes of He gas flow. These fuel elements are located in a reactor water pool of atmospheric pressure (0.1 MPa) and low temperature (<60 °C). In case of LOF, decay heats of fuel elements are removed by natural heat transfer from surfaces of the fuel elements to the reactor water pool.

Preliminary neutronic calculations of the “METAL-KAMADO” show possibility of high burn-up of more than 120 GWd/t with 10% enriched U–Zr fuel. Reactivity coefficients of the core are also discussed.     

Trace elements in sera from patients with renal disease

In hemodialysis (HD) patients, an accumulation of trace elements such as aluminum, copper, silicon and vanadium has been reported. Aluminum-caused encephalopathy and aluminum-related bone diseases are important trace element-related complications. Using particle induced X-ray emission (PIXE) we determined concentrations of aluminum, silicon, copper, zinc, selenium and bromine in sera of 29 patients with HD, 14 nondialysis patients with renal disease (RD) and 27 normal controls. The concentration of serum silicon of the patients with HD was 107.4 ± 61.3 μmol/l, which is markedly higher than that of normal controls (48.3 ± 25.8 μmol/l, p < 0.0001). The serum concentrations of zinc and bromine in patients with HD were 11.9 ± 1.7 and 21.3 ± 3.0 μmol/l, respectively. Both were markedly lower than those of normal controls (15.6 ± 2.6, 69.2 ± 8.3 μmol/l, p < 0.0001). The concentrations of aluminium and bromine in the serum of patients with RD were 171.9 ± 64.3 and 81.9 ± 11.6 μmol/l, which were markedly higher than those of normal controls (p < 0.0001, p < 0.001). No significant differences were observed in the concentration of copper and selenium among three groups.     

EDXRF analysis of Marajoara pubic covers

This work evaluated the elemental composition of decorated pottery pubic covers (tangas) from the Marajoara culture of Marajó Island (at the mouth of the Amazon River, Brazil) using EDXRF technique. The XRF system used in this work consists in a Si(Li) detector from ORTEC, with resolution of 180 eV, at 5.9 keV, and a mini X-ray tube with Mo anode. The elements identified in the samples were: S, Cl, K, Ca, Ti, Mn, Fe, Cu, Zn, Ga, Rb, Sr, Y, Zr and Pb. Principal components analysis (PCA) was used to evaluated the provenance of the samples.     

Structure and optical properties of sapphire implanted with boron at room temperature and 1000 °C

Many previous studies of ion-implanted sapphire have used gas-forming light ions or heavier metallic cations. In this study, boron (10¹⁷ cm⁻², 150 keV) was implanted in c-axis crystals at room temperature, 500 and 1000 °C as part of a continuing study of cascade density and “chemical” effects on the structure of sapphire. Rutherford backscattering-ion channeling (RBS-C) of the RT samples indicated little residual disorder in the Al-sublattice to a depth of 50–75 nm but almost random scattering at the depth of peak damage energy deposition. The transmission electron micrographs contain “black-spot” damage features. The residual disorder is much less at all depths for samples implanted at 1000 °C. The TEM photographs show a coarse “black-spot damage” microstructure. The optical absorption at 205 nm is much greater than for samples implanted with C, N, or Fe under similar conditions.     

Brain trace elements and aging

Degenerative mechanisms involved in the aging process of the brain are to a certain extent counteracted by repair mechanisms. In both degenerative and recovery processes, trace elements are involved. The present study focused on the role of two minor (i.e., K and Ca) and six trace elements (i.e., Mn, Fe, Cu, Zn, Se and Rb) in the aging process. The elements were determined by PIXE in cerebral cortex and white matter, basal ganglia, brainstem and cerebellar cortex of 18 postmortem human brains, from persons without a history of neurologic or psychiatric disease who deceased between the age of 7 and 79. This age range allowed us to study the relationship between elemental concentrations and age. The most prominent findings were a concentration decrease for K and Rb and a concentration increase for the elements Ca, Fe, Zn and Se. The study supports recent findings that Ca and Fe are involved in brain degenerative processes initiated by oxygen free radicals, whereas Zn and Se are involved in immunological reactions counteracting the aging process.     

Evaluation of elemental status of ancient human bone samples from Northeastern Hungary dated to the 10th century AD by XRF

The present study is a multielemental analysis of bone samples belonging to skeletal individuals originating from two contemporaneous (10th century AD) cemeteries (Tiszavasvári Nagy-Gyepáros and Nagycserkesz-Nádasibokor sites) in Northeastern Hungary, using the XRF analytical technique. Emitted X-rays were detected in order to determine the elemental composition of bones and to appreciate the possible influence of the burial environment on the elemental content of the human skeletal remains. Lumbar vertebral bodies were used for analysis. Applying the ED(P)XRF technique concentration of the following elements were determined: P, Ca, K, Na, Mg, Al, Cl, Mn, Fe, Zn, Br and Sr. The results indicated post mortem mineral exchange between the burial environment (soil) and bones (e.g. the enhanced levels of Fe and Mn) and referred to diagenetic alteration processes during burials. However, other elements such as Zn, Sr and Br seemed to be accumulated during the past life. On the basis of statistical analysis, clear separation could not be observed between the two excavation sites in their bone elemental concentrations which denoted similar diagenetic influences, environmental conditions. The enhanced levels of Sr might be connected with the past dietary habits, especially consumption of plant food.     

Enthalpy and heat capacity of LiAlO2 between 298 and 1700 K by drop calorimetry

The enthalpy of γ-LiAlO₂ was measured between 403 and 1673 K by isothermal drop calorimetry. The smoothed enthalpy curve between 298 and 1700 K results in H⁰(T) − H⁰(298 K)=−37 396 + 93.143 · T + 0.00557 · T² + 2 725 221 · T⁻¹ J/mol. The standard deviation is 2.2%. The heat capacity was derived by differentiation of the enthalpy curve. The value extrapolated to 298 K is C_p,298=(65.8 ± 2.0) J/K mol.     

Elemental investigation of Syrian medicinal plants using PIXE analysis

Particle induced X-ray emission (PIXE) technique has been employed to perform elemental analysis of K, Ca, Mn, Fe, Cu, Zn, Br and Sr for Syrian medicinal plants used traditionally to enhance the body immunity. Plant samples were prepared in a simple dried base. The results were verified by comparing with those obtained from both IAEA-359 and IAEA–V10 reference materials. Relative standard deviations are mostly within ±5–10% suggest good precision. A correlation between the elemental content in each medicinal plant with its traditional remedial usage has been proposed. Both K and Ca are found to be the major elements in the samples. Fe, Mn and Zn have been detected in good levels in most of these plants clarifying their possible contribution to keep the body immune system in good condition. The contribution of the elements in these plants to the dietary recommended intakes (DRI) has been evaluated. Advantages and limitations of PIXE analytical technique in this investigation have been reviewed.     

骨骼样品PIXE分析测定方法研究

简单介绍用内标法测定骨骼样品中微量元素的制样方法，特别是复合吸收片的方法，可克服主量元素Ｐ和Ｃａ对微量元素的影响，使骨骼样品的质子激发Ｘ荧光分析法（ＰＩＸＥ）能谱中微量元素Ｓ、Ｋ、Ｓｃ、Ｖ、Ｃｒ、Ｍｎ、Ｃｏ、Ｃｕ、Ｚｎ的能峰清晰、突出，为定量分析奠定了基础。微量元素Ｆｅ和Ｓｒ的相对规一含量在骨折愈合过程中分别呈鼓凸形和下凹形规则性变化。     

Post-irradiation mechanical properties of three EUROFER97 joints

Within the development of reduced activation ferritic martensitic (RAFM) steels as prominent structural materials for future fusion reactors, EUROFER97 has recently emerged in Europe as the reference material for the DEMO design. In order to characterise the in-service performance of EUROFER97 as structural material, it is important to assess the properties of welded joints, particularly under irradiation. In the present paper, three EUROFER97 joints (two diffusion welds and one TIG weld) have been irradiated in the BR2 reactor of SCK-CEN at 300 °C up to 1.8 dpa and subsequently characterised for tensile, impact and fracture toughness properties. Comparisons of the results are provided with base EUROFER97 (both unirradiated and irradiated under similar conditions) and, where available, with properties measured on the joints in the unirradiated condition. The post-irradiation mechanical behaviour of both diffusion joints (“laboratory” and “mock-up”) appears similar to that of the base material; therefore, diffusion joining looks a very promising technique. On the other hand, the properties of the TIG joint are affected by the lack of a post-weld heat treatment, which causes the material from the upper part of the weld to be significantly worse than that of the lower region.     

Determination of stoichiometry in silicon carbide materials using elastic backscattering spectrometry

Elastic backscattering spectrometry (EBS) was performed on SiC materials, using ⁴He particles at energies ranging from 2 to 4 MeV, in order to establish the energy values that lead to an accurate measurement of the Si/C ratio. Analysis of the random yield of “bulk” SiC single crystals indicates that energy values of 3.25 and 3.75 MeV are the most suitable for chemical composition determination; backscattering yield of carbon is enhanced compared to the yield measured at 2 MeV, while the excitation of strong resonances above 3.75 MeV are suppressed. Random backscattering yield measurements were then carried out at an energy of 3.25 MeV on unhydrogenated SiC thin films grown on Si(1 0 0), by pulsed laser deposition, at different substrate temperatures. The Si and C atomic concentrations in the films were determined with an uncertainty of 1% and little interference from the underlying substrate. The films were found to be stoichiometric with a Si/C ratio of 1.03 ± 0.05, independent of deposition temperature, which indicates that the films were grown under congruent ablation conditions. The analysis proved to be applicable to both amorphous and crystalline SiC layers, as confirmed by the results obtained for films deposited at 400 and 950 °C, respectively.     

EDXRF analysis of beach rock samples of Andaman Island

B Elemental contents of beach rock samples were analyzed using EDXRF. The samples were collected from three locations of Andaman Island. The Al, Ca, K, Fe, Ti, Si, V, Co, Cu, Ba, Zn, Ph, Cd and Mn contents were determined. The geochemical behavior of elements in the region is discussed. The elemental contents of beach rock samples from Andaman Island are much below the values of both earth crust and that of Tamilnadu region. However,content of the biogenic element Ca was the highest of all dements. This is due to the typical beach rock formation.     

Trace elements of soil samples from mining area

The affect of mining activity on the environment has been long of public concern. The present paper deals with the elemental analysis of soil samples from a mine and the area around it, located in E 48°59′ and N 34°11′ in Hamadan province of Iran. Elemental analysis was done using Proton Induced X-ray Emission (PIXE) technique. Spectra analysis and quantification was done using GUPIX software. Besides the major elements Si, P, K, Ca, Mn and Fe the other elements, namely Cl, Ti, V, Cr, Co, Ni, Cu, Zn, Rb, Sr and Pb were also present. Arsenic could be detected in some samples only. The presence of Ba and Ce needs more investigations by other techniques due to overlap of the L X-rays of these elements with the K X-rays of the major elements Mn and Fe, etc. Many elements V, Cr, As and Pb are known to be toxic and needs further understanding and proper handling in the mining process.     

PIXE analysis of ancient Chinese Changsha porcelain

In this work, proton induced X-ray emission (PIXE) method was applied for the analysis of ancient Chinese Changsha porcelain produced in the Tang dynasty (AD 618–907). A collection of glazed potsherds was obtained in the complex of the famous kiln site at Tongguan, Changsha city, Hunan province. Studies of elemental composition were carried out on ten selected Changsha potsherds. Minor and trace elements such as Ti, Mn, Fe, Co, Cu, Rb, Sr, and Zr in the material of the porcelain glaze were determined. Variation of these elements from sample to sample was investigated. Details of results are presented and discussed.     

Elemental analysis of edible grains by micro-PIXE: Common buckwheat case study

The aim of this study was the adaptation of the micro-PIXE method for analysis of nutritionally relevant heavy elements in different tissues of the grain of common buckwheat (Fagopyrum esculentum), as a representative nutritionally interesting grain food source. At 57% of the buckwheat grain biomass, the endosperm was a modest nutrient source when compared to the cotyledons, at 17% of the biomass. These latter contained high concentrations of trace elements, representing 91% of the total grain Zn, 87% for P, 70% for S, 62% for Mg, 60% for K, 54% for Cu, 53% for Mn and 35% for Fe. The husk provided storage for 85% of the total Ca, 84% for Al, 83% for Si, 76% for Cl, 69% for Ti and 46% for Fe. Knowledge on these preferential elemental constitutions of the different grain tissues makes the possibility of designing target products with nutritionally optimal constitution more feasible. These data represent a basis for a more targeted approach to nutritional improvement of grains intended for human consumption.     

Application of micro-PIXE,MRI and light microscopy for research in wood science and dendroecology

Beech (Fagus sylvatica L.) branches were topped and after five months the wound response was analyzed by PIXE, 3D-MRI and light microscopy. From freshly cut and deeply frozen sample 30 μm thick longitudinal-radial tissue sections were prepared for anatomical investigations and micro-PIXE analysis. Light microscopy revealed the structural response to wounding, i.e. occurrence of the reaction zone between the exposed and dehydrated dead tissue and healthy sound wood. The reaction zone was characterized by tylosis in vessels and accumulation of colored deposits in parenchyma cells, fibres and vessels. 3D MRI of a parallel sample showed that the moisture content in the reaction zone was three times higher than in normal healthy wood. Micro-PIXE mapping at margins of compromised wood in beech revealed an increased concentration of potassium in the reaction zone. The increase in the calcium concentration was associated with the dehydrated tissue adjacent to reaction zones.In addition, micro-PIXE was used to determine the elemental distribution in annual tree rings. This may be relevant for retrospective assessment of environmental pollution in wood by measuring yearly increments as a biomonitoring tool. The analysis of European larch (Larix decidua Mill.) wood revealed a high similarity between optical characteristics (i.e. late versus earlywood) and elemental (e.g. Cl, K, Ca, Mn, Zn) distribution.     

Spin-resolved magnetic studies of focused ion beam etched nano-sized magnetic structures

Scanning ion microscopy with polarization analysis (SIMPA) is used to study the spin-resolved surface magnetic structure of nano-sized magnetic systems. SIMPA is utilized for in situ topographic and spin-resolved magnetic domain imaging as well as for focused ion beam (FIB) etching of desired structures in magnetic or non-magnetic systems. Ultra-thin Co films are deposited on surfaces of Si(1 0 0) substrates, and ultra-thin, tri-layered, bct Fe(1 0 0)/Mn/bct Fe(1 0 0) wedged magnetic structures are deposited on fcc Pd(1 0 0) substrates. SIMPA experiments clearly show that ion-induced electrons emitted from magnetic surfaces exhibit non-zero electron spin polarization (ESP), whereas electrons emitted from non-magnetic surfaces such as Si and Pd exhibit zero ESP, which can be used to calibrate sputtering rates in situ. We report on new, spin-resolved magnetic microstructures, such as magnetic “C” states and magnetic vortices, found at surfaces of FIB patterned magnetic elements. It is found that FIB milling has a negligible effect on surface magnetic domain and domain wall structures. It is demonstrated that SIMPA can evolve into an important and efficient tool to study magnetic domain, domain wall and other structures as well as to perform magnetic depth profiling of magnetic nano-systems to be used in ultra-high density magnetic recording and in magnetic sensors.     

Enthalpies of formation of U-, Th-, Ce-brannerite: implications for plutonium immobilization

Brannerite, ideally MTi₂O₆, (M=actinides, lanthanides and Ca) occurs in titanate-based ceramics proposed for the immobilization of plutonium. Standard enthalpies of formation, ΔH⁰_f at 298 K, for three brannerite compositions (kJ/mol): CeTi₂O₆ (−2948.8 ± 4.3), U_0.97Ti_2.03O₆ (−2977.9 ± 3.5) and ThTi₂O₆ (−3096.5 ± 4.3) were determined by high temperature oxide melt drop solution calorimetry at 975 K using 3Na₂O · 4MoO₃ solvent. The enthalpies of formation were also calculated from an oxide phase assemblage (ΔH⁰_f-ox at 298 K): MO₂ + 2TiO₂=MTi₂O₆. Only UTi₂O₆ is energetically stable with respect to an oxide assemblage: U_0.97Ti_2.03O₆ (ΔH⁰_f-ox=−7.7±2.8 kJ/mol). Both CeTi₂O₆ and ThTi₂O₆ are higher in enthalpy with respect to their oxide assemblages with (ΔH⁰_f-ox=+29.4±3.6 kJ/mol) and (ΔH⁰_f-ox=+19.4±1.6 kJ/mol) respectively. Thus, Ce- and Th-brannerite are entropy stabilized and are thermodynamically stable only at high temperature.     

PIXE analysis of trace elements in northern fur seal teeth

Trace elements in teeth of northern fur seal Collorhinus ursinus were analyzed by PIXE and micro-PIXE (μ-PIXE). Trace elements such as Mn, Fe, Zn, Cu, As, Br, Sr, and Pb were detected in the teeth, which were composed of hydroxyapatite crystals. Among these elements, the concentrations of Fe and Zn were relatively higher in winter and lower in summer and also Zn varied along with growth of individuals. These elemental fluctuation seems to correspond to the life history of the northern fur seal. It suggests that the PIXE analysis will make a powerful tool to reconstruct the life history.