This paper details an improved approach to environmental particle analysis for safeguards by means of a combination of an upgraded version of the so-called fission track method with state-of-the-art microscope and microprobe techniques. Improvements to the fission track method comprise a novel sample assembly, the automation of several of its steps and the extensive use of correlative microscopy. This is followed by an automated isolation of particles-of-interest by means of laser micro-dissection (LMD) and their collection onto a harvester for transfer to other micro-analytical instruments for further analysis. The samples examined in this contribution were analysed for their nuclear material signatures, in particular the presence of uranium isotopes. The length of a single analysis cycle herewith was reduced to 12 days.

A long-standing question in morphological evolution is why male genitalia tend to diverge more rapidly than other structures. One possible explanation is that male genitalia are under sexual selection to function as ‘internal courtship devices’. Males of closely related species may provide divergent stimulation using different genital morphologies and behaviors. Testing this hypothesis has been difficult, however, because the presumed genital courtship behavior is often hidden from view inside the female, and because studies of how the male’s genitalia interact with those of the female are nearly always limited to a single species in a given group, thus restricting opportunities for comparison of closely related species. We present new morphological and behavioral data for portions of the male genitalia that are hidden in the female during copulation in five species in the tsetse fly genus Glossina using data from dissections of pairs frozen in copula, artificially stimulated males, and from copulating pairs viewed with a new X-ray technique that allows events inside the female to be recorded in real time. These data almost certainly give only an incomplete view of this complex, previously hidden world. But even so they clearly reveal that, as predicted by sexual selection theory, the male genitalia of Glossina flies perform dramatic, stereotyped, rhythmic movements deep within the female’s reproductive tract and in inward folds of her external surface, and that many of these movements probably differ among closely related species. Most of the movements are not explicable as means by which the male anchors himself more securely to the female; all are likely to result in stimulation of the female. A female Glossina can be stimulated tactilely at a given moment during copulation at up to 8–10 or more different sites on her body.

This paper presents a novel approach to environmental particle analysis for safeguards by means of a combination of micro-analytical techniques. It includes the tandem utilization of two separate light microscopes, a scanning electron microscope and a femtosecond laser-ablation ICP-MS. These are: a light microscopy automated particle relocation device (Zeiss Z2m); an optical-microscopy-based laser micro-dissection system (IX83 MMI+Olympus); a focussed ion beam scanning electron microscope equipped with a time-of-flight mass spectrometer extension (Tescan Lyra3) and a fs LA-ICP-MS (J200 from Applied Spectra Inc. and Thermofisher Scientific iCap Q). The samples examined in this contribution are analysed for their nuclear material signatures, in particular the presence of uranium isotopes.

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A portable focused-beam X-ray fluorescence (XRF) spectrometer was designed and manufactured taking into account a huge variation in material, size and shape of museum objects. The spectrometer is equipped with a vacuum chamber enclosed with a Kapton-window allowing the detection of chemical elements from Na upwards, which enables the characterization of glass and enamel objects. Two low-power X-ray tubes, one with a Mo-anode the other with a Cr-anode, operating from 4 to 50 kV and 0 to 2.5 mA with a maximum power of 50W and a point focus of about 180 mu m can be used as excitation source alternatively. A polycapillary lens with a spot size of 150 mu m is used for focusing the primary beam to access small details of the different objects, e.g. fine brush strokes in paintings. The vacuum chamber can be evacuated to about 1 mbar.A miniature camera is installed inside the chamber for inspecting the analyzed area through the Kapton-window. Two laser pointers mounted inside the chamber coincide with the focal point of the polycapillary at the investigated spot. The excitation and X-ray fluorescence radiation paths in air are about 1 mm each, minimizing the absorption losses. The spectrometer was designed to maximize the accessibility to all parts of the investigated objects through the use of translation stages and an innovative design of the detection head, especially the vacuum chamber. This article shows the capability of the spectrometer to reach measuring positions in concave parts of objects and presents the determined detection limits of elements. Copyright (C) 2009 John Wiley & Sons, Ltd.

Shon (2009, Ethology Ecology Evolution 21: 161-172) pointed out that in order to understand the functional morphology of sexually selected structures that are used as signaling devices in birds, it is crucial to understand how these structures move during sexual interactions. This insight applies not only to bird feathers, but also to many other types of possible signaling devices, including male genitalia. This note highlights the need for studies of the behavior of genitalia, and describes two promising techniques, using a tsetse fly as an example. Observations of this species revealed otherwise cryptic, highly rhythmic and forceful thrusting, pinching, pressing, and scraping movements by the male's genitalia within the female's body that have no obvious relation to sperm transfer. Thus even though on the outside the male`s body is nearly motionless during long lapses during copulation, the female is subject to a barrage of possible stimulation from his genitalia during copulation. Similar studies are needed in other groups to understand the functional significance of genital morphology.

X-ray emission techniques play important role in the cultural heritage area. They provide information about chemical composition of an object upon bombardment of its surface with electrons, ions, or electromagnetic radiation. Their useful features include non-destructiveness, multielemental capability, and high sensitivity for inorganic components. Especially widely used is the X-ray fluorescence technique. It utilizes electromagnetic radiation generated by X-ray tubes or radioisotope sources. X-ray fluorescence equipment is relatively simple as compared to the charged particle-based spectrometers which are combined with scanning electron microscope or ion beam accelerator. X-ray fluorescence technique can be easily adapted for in situ measurements. A portable X-ray fluorescence spectrometer has been constructed utilizing commercially available, ready made components. The construction details of the spectrometer and examples of its application are given. The key features of the portable system are the use of polycapillary X-ray optics and a vacuum chamber attachment to enhance detection of low atomic number elements such as Mg, Al, Si, P, S, and Cl. The spectrometer was applied for chemical composition analysis of archaeological artifacts and works of arts from the collections of the Museum of Fine Arts (Kunsthistorisches Museum), Vienna, Austria. The investigated objects included ancient bronzes, coins, samples of pigments, and famous goldsmith work "Saliera" by Benvenuto Cellini (1500-1571). This work highlights also other projects related to the applications of nuclear analytical techniques in support of study and preservation of cultural heritage objects supported by the International Atomic Energy Agency and carried out in the Agency's Member States.

The performance of x-ray capillary lenses has been evaluated. The tests were carried out using an x-ray tube set-up. A single glass capillary with tapered inner channel, a monolithic glass polycapillary, and an in-house manufactured single metallic capillary with parabolic inner channel were characterized in terms of gain, spatial resolution, and element detection limits. The spatial resolution of a confocal set-up utilizing a monolithic glass polycapillary and a polycapillary conical collimator has also been measured. The highest gain of about 2500 was observed for the glass polycapillary. The maximum gain achieved with the single glass capillary was equal to about 25, and the gain of the metallic capillary was only slightly greater than 1. For the glass capillary and polycapillary lenses, significant filtering of the higher.. energy photons (energy >8 keV) was observed. The lowest relative detection limits were obtained with an ordinary cylindrical collimator and the polycapillary lens. Similar absolute detection limits were achieved with the use of the polycapillary and single capillary lenses. A relation between the ratios of the detection limits of elements achieved with different x-ray lenses and the lens parameters (spatial resolution and gain) has been proposed and was verified experimentally. The monolithic polycapillary lens was found to be an optimum focusing device for an x-ray tube-based scanning spectrometer. This type of x-ray lens. can be coupled with a polycapillary conical collimator or a polycapillary half-lens to make a confocal x-ray microscope capable of depth profiling with a spatial resolution equal to about 30 micrometers. Copyright (C) 2008 John Wiley & Sons, Ltd.

X-ray fluorescence analysis (XRF) is a powerful tool for nondestructive analysis of chemical elements present in art and archeological material. Nevertheless, investigations of objects possessing a glassy matrix still offer some problems using XRF because of the absorption in air of the low-energy characteristic fluorescence radiation of light elements. With the design of a XRF instrument equipped with a vacuum chamber housing both, the x-ray optics and the detector snout inside, a new attempt to solve this problem was made. The Conservation Science Department of the Kunsthistorisches Museum Vienna (KHM) had the opportunity to test this instrument on different objects of art. An overview of some results from these measurements, together with a short discussion of the experiences gained during the investigations, is presented in this article. Copyright  2008 John Wiley & Sons, Ltd.

1) Agency’s Laboratories Seibersdorf, International Atomic Energy Agency, A-1400 Vienna, Austria 2) Faculty of Physics and Applied Computer Science, University of Science and Technology, 30-059 Krakow, Poland 3) Atominstitut der Oesterreichischen Universitaeten, TU Wien, Stationallee 2, A-1020 Vienna, Austria 4) Forschungszentrum Karlsruhe, Institute for Synchrotron Radiation, Postfach 3640, D-76021 Karlsruhe, Germany

Based on the design of the low cost Total Reflection X-Ray Fluorescence attachment module available since 1986 from Atominstitut (WOBRAUSCHEK-module) which can be attached to existing X-ray equipment, a new version was developed which allows the analysis of samples in vacuum. This design was in particular possible as the Peltier cooled light weight Silicon Drift Detector is following all adjustment procedures for total reflection as angle rotation and linear motion. The detector is mounted through a vacuum feed and O-ring tightening to the small vacuum chamber. The standard 30 mm round quartz, Si-wafer or Plexiglas reflectors are used to carry the samples. The reflectors are placed on the reference plane with the dried sample down looking facing in about 0.5 mm distance the up looking detector window. The reflectors are resting on 3 steel balls defining precisely the reference plane for the adjustment procedure. As the rotation axis of the module is in the plane of the reflector surface, angle dependent experiments can be made to distinguish between film and particulate type contamination of samples. Operating with a Mo anode at 50 kV and 40 mA with a closely attached multilayer monochromator and using a 10 mm(2) KETEK silicon drift detector with 8 pm Be window, a sensitivity of 70 cps/ng for Rb was measured and detection limits of 2 pg were obtained. (C) 2008 Elsevier B.V. All rights reserved.

In humans the toxic trace element lead (Pb) mainly accumulates in the skeletal tissue where it resides for a long period. Although Pb is known to play a role in bone and cartilage diseases, the distribution Of Pb in these tissues is mostly unknown. Therefore synchrotron-radiation-induced micro x-ray fluorescence analysis (SR mu-XRF) in various geometries was used to determine the distributions of Pb, Ca, Zn and Sr at the cartilage-bone interface in human femoral heads and patellae. SR mu-XRF results were matched with backscattered electron (BE) images providing information on structural features of the tissue. Conventional SR mu-XRF at HASYLAB beamline L showed that Pb mostly accumulates in a zone of some micrometers around the transition between non-calcified and calcified cartilage. However, the relatively large sample thickness did not allow more precise conclusions. Exploiting the 3D capabilities of confocal SR mu-XRF and SR microfluorescence tomography at ANKA Fluo-Topo beamline and HASYLAB beamline L, the spatial resolution could be improved and a highly specific accumulation of Pb at the tidemark, the calcification front between non-calcified and calcified cartilage, was detected. It was found that Pb and Zn accumulation coincide at the tidemark. Since the tidemark plays an important role in osteoarthritis, the results may strengthen other authors' conclusions that Pb is associated with this joint disease. Although offering less spatial resolution when compared to micro-tomography, confocal SR mu-XRF is best suited for such studies. It facilitates the comparison of element maps with other imaging techniques like BE imaging. Copyright (C) 2007 John Wiley & Sons, Ltd.

A portable focused-beam XRF spectrometer was designed, constructed, and manufactured. The spectrometer allows to detect and perform analysis of chemical elements from Na upwards. The system is equipped with a compact vacuum chamber to reduce absorption of both the excitation and the fluorescence radiation in air. A low power Pd-anode tube operated up to 50 kV and 1 mA with a point focus of 400 mu m is used as excitation source. A polycapillary lens with a spot size of about 160 pm, or a collimator with a 1 min inner diameter can be used alternatively for either focusing or collimating the primary beam. The fluorescence radiation is collected by an Si drift detector with an active area of 10 min 2 and equipped with an 8 mu m Be entrance window.A compact vacuum chamber was designed to house the X-ray beam optics and the detector snout. The chamber is attached to the X-ray tube and can be pumped down to 0.1 mbar. A Kapton(TM) window of 7.5 mu m thickness allows to locate the investigated spot at about 1-2 mm distance outside of the chamber, thus minimizing absorption losses in the excitation and X-ray fluorescence radiation paths. Two lasers pointers are mounted inside the chamber. The laser beams cross at a point outside the chamber in front of the entrance window and coincide with the focal spot of the polycapillary.This paper reports some preliminary results obtained from an in situ analysis of bronze samples as well as a comparison of these data with those given by other laboratory spectrometers and the reference values provided by the Italian bronze foundry Venturi Arte Bologna, Italy. (C) 2007 Elsevier B.V. All rights reserved.

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A method of correction for absorption effects in micro-beam x-ray fluorescence analysis is described. A fast, energy-dispersive, silicon drift detector (SDD) was used to measure the primary x-ray beam transmitted through the sample. The absorption factors were calculated using the data acquired with the SDD. The possibility of using the coherently, incoherently and multiple scattered primary radiation for determining the mass of individual particles was examined. The proposed methods were validated with the use of NIST K3089 glass micro-spheres of known composition. Copyright (C) 2006 John Wiley & Sons, Ltd.

This paper describes the specific philosophy behind the functioning of the IAEA XRF Laboratory at Seibersdorf and its role in the XRF community. Some examples of the research and development activities and the results obtained are given. They include methodological development and construction of XRF instruments in order to extend the applicability range of the XRF technique, particularly in support of applications of the analytical technique in developing IAEA member states. The contribution of the laboratory to the training in methodology and applications of XRF techniques and to development of QA/QC procedures is also emphasised. Copyright © 2006 John Wiley & Sons, Ltd.

Six radioactive particles stemming from Thule area (NW-Greenland) were investigated by gamma-ray and L X-ray spectrometry based on radioactive disintegration, scanning electron microscopy coupled with energy-dispersive and wavelength-dispersive X-ray spectrometer, synchrotron radiation based techniques as microscopic X-ray fluorescence, microscopic X-ray absorption near-edge structure (μ-XANES) as well as combined X-ray absorption and fluorescence microtomography. Additionally, one particle from Mururoa atoll was examined by microtomography. From the results obtained, it was found out that the U and Pu were mixed in the particles. The U/Pu intensity ratios in the Thule particles varied between 0.05 and 0.36. The results from the microtomography showed that U/Pu ratio was not homogeneously distributed. The 241Am/238+239+240Pu activity ratios varied between 0.13 and 0.17, indicating that the particles originate from different source terms. The oxidation states of U and Pu as determined by μ-XANES showed that U(IV) is the preponderant species and for Pu, two types of particles could be evidenced. One set had about 90% Pu(IV) while in the other the ratio Pu(IV)/Pu(VI) was about one third.