Performance of polycapillary x‐ray lens for x‐ray sources with various spot sizes

The performance of a polycapillary x‐ray lens (PCXRL) is related to the spot size of the x‐ray source. The transmission efficiency of the PCXRL decreases generally with the increase of the x‐ray source spot size. Both the output focal spot size of a focusing PCXRL and the divergence of a parallel PCXRL increase with increasing source spot size. A large source spot size results in more ‘escape halo’, which affects the measured transmission efficiency and the measured output focal spot size. Copyright © 2007 John Wiley & Sons, Ltd.     

Calculation of the transmission efficiency of a monolithic polycapillary x‐ray lens for an x‐ray source of any shape

A method for calculating the transmission efficiency of a monolithic polycapillary x‐ray lens is presented. Using this method, the transmission efficiency of an x‐ray source of any shape can be calculated by using the transmission efficiency measured with a microfocus x‐ray source. Copyright © 2005 John Wiley & Sons, Ltd.     

Portable x‐ray fluorescence spectrometer with a pyroelectric x‐ray generator

A portable x‐ray fluorescence spectrometer was assembled with an x‐ray generator that was driven by a 9 V dry electric battery. Several possible optimum geometries of the x‐ray generator and detector were evaluated, and the results showed that the intensity of fluorescent x‐rays was strong enough when the angle between the x‐ray generator and detector was as small as 30°. The geometrically optimized x‐ray spectrometer was applied to the analysis of paints, plastics and aluminum foils. Pigments in paint and toxic elements in plastic could be easily detected with on‐site analysis. Fe in aluminum foil was quantitatively determined down to the sub‐% level. The detection limit of Fe was 180 ppm for 100 s of measurement. Copyright © 2005 John Wiley & Sons, Ltd.     

The capabilities of an electrically cooled energy‐dispersive x‐ray detector for quantitative x‐ray fluorescence analysis

The capabilities of the Si PIN diode x‐ray detector were determined and compared with those of a standard Si(Li) detector. The x‐ray fluorescence (XRF) analysis systems assembled with these two detectors included annular radioisotope excitation sources of Cd‐109 and Fe‐55. The systems were calibrated for sensitivity and quantification was performed with fundamental parameters software. Based on the analysis of the standard reference material NIST 2710 (Montana soil), the elemental sensitivities and the limits of detection of both systems were obtained. The elemental sensitivities of the Si PIN detector for fluorescence x‐rays in the energy range up to 10 keV were comparable to those of the Si(Li) detector. At higher fluorescence x‐ray energies the sensitivity of the Si PIN detector gradually decreased and was smaller by a factor of ～4 at 20 keV. The reason was mainly the small thickness of the sensitive volume of the Si PIN diode (0.2 mm) and therefore the smaller relative efficiency of this detector. The assessed limits of detection (LODs) were comparable for the two detectors, which was mainly due to the lower spectral background of the Si PIN detector in excitation with the Cd‐109 source as a result of its smaller sensitive thickness. The accuracy of elemental determinations for the two detectors was comparable and within the limits of the assessed uncertainties, which were calculated considering all the steps of the analysis, i.e. spectrum measurement and analysis, sensitivity calibration and quantification. Copyright © 2004 John Wiley & Sons, Ltd.     

Calculation of attenuation and x‐ray fluorescence intensities for non‐parallel x‐ray beams

With the nowadays widespreaded use of x‐ray optics in x‐ray fluorescence analysis, large convergence or divergence angles can occur. This experimental situation violates a basic assumption of the usual fundamental parameter quantification procedure. In order to take beam divergences in micro x‐ray fluorescence analysis into account, a way of calculating fluorescence intensities numerically by Monte Carlo integration is described. For three examples of typical micro‐XRF set‐ups the fluorescence intensities and their deviation from the parallel beam geometry are calculated. Furthermore, we propose a new approach with ‘equivalent angles’ which correct for the beam divergences in fundamental parameter methods. Copyright © 2003 John Wiley & Sons, Ltd.     

Short soft x‐ray sources

In this work we report on the characterization of pulsed soft x‐rays emitted from laser‐produced plasma. The plasma was generated by a pulsed KrF excimer laser focused on pure Si, Cu and Ta targets by 40, 80 and 120 mJ laser energies. The utilized detector was a very sensitive Faraday cup which opportunely biased was able to record time‐resolved signals of x‐rays and to estimate their energy. The found x‐rays energy values were compared with the ion temperature of the plasma obtained by fitting the time‐resolved ion current signals with a shifted Maxwell‐Boltzmann velocity distribution. The results showed that the laser‐produced Ta plasma induced bunches of x‐rays having in average the highest energy values and it was also characterized by ion temperature higher than the ones of the laser‐produced Si and Cu plasmas. Copyright © 2009 John Wiley & Sons, Ltd.     

Characterization of homemade x‐ray polycapillaries

The possibilities of performing non‐destructive elemental microanalysis with synchrotron radiation by means of homemade polycapillary optics are described. Using fiber glass technology, monolithic polycapillary half‐lenses were made by drawing packages of glass capillaries at high temperature in a heating furnace. The performance of polycapillary half‐lenses with different geometries was evaluated. A gold knife‐edge scanned at the output of the lenses was used to determine the spot size at different distances. Measurements of photon flux impinging on the entrance end of the lenses and photon flux leaving the lenses were used to obtain the transmission efficiency. The polycapillary half‐lens made in our laboratory was used in a series of XRF microanalysis tests using white beam. The overall efficiency of the system was studied by means of establishing detection limits for various elements in an organic sample. Copyright © 2008 John Wiley & Sons, Ltd.     

X‐ray fluorescence analysis with a pyroelectric x‐ray generator

Several types of handy x‐ray fluorescence spectrometers are presented. The results obtained with a Niton spectrometer are presented as a goal to develop a laboratory‐made spectrometer using an Amptek Cool‐X pyroelectric x‐ray generator. A small and cheap charge‐up x‐ray emitting device and its spectrum are also presented. Handy x‐ray spectrometers are now progressing rapidly and the detection limits are in the range of a few ppm for certain elements. Copyright © 2005 John Wiley & Sons, Ltd.     

HOPG as powerful x‐ray optics

A new method of producing strongly bent highly oriented pyrolytic graphite (HOPG) is presented. The method allows one to make a crystal of almost arbitrary shape, but has some thickness limits. A review of the results obtained on this type of crystal by different laboratories during the last 10 years is given. An x‐ray intensity gain from a synchrotron radiation source and Mo Kα tube beams of one order of magnitude could be achieved when using a crystal of optimized shape. The application of the crystals for secondary monochromatization in EDXRF improves by one order of magnitude the detection limits for the elements of interest. Copyright © 2003 John Wiley & Sons, Ltd.     

Active region of x‐ray emission

The active region of x‐ray emission was studied. The x‐ray emission rates for K and L x‐rays were calculated as a function of the maximum radial distance in integration of matrix elements for radiative transitions and the radius of the active region of x‐ray emission was determined. This radius depends on the multipolarity of the transition and also the sum of numbers of nodes of the wavefunctions concerned. The approximate expression for the radius of the active region is obtained in terms of the mean radius of the wavefunction for the initial vacancy state. Applications of the present results to multiple ionization and to chemical effects are discussed. Copyright © 2005 John Wiley & Sons, Ltd.     

A desktop X‐ray monochromator for synchrotron radiation based on refraction in mosaic prism lenses

Focusing planar refractive mosaic lenses based on triangular prism microstructures have been used as an alternative approach for wide‐bandpass monochromatization of high‐energy X‐rays. The strong energy dependence of the refractive index of the lens material leads to an analogous energy dependence of the focal length of the lens. The refractive mosaic lens, in comparison with the refractive lens of continuous parabolic profile, is characterized by a higher aperture because of reduced passive material. In combination with a well defined pinhole aperture in the focal plane, the transmittance of photons of an appropriate energy can be relatively high and photons of deviating energy can be efficiently suppressed. The photon energy can be tuned by translating the pinhole along the optical axis, and the bandwidth changed by selecting appropriate pinhole aperture and beam stop. This method of monochromatization was realised at the ANKA FLUO beamline using a mosaic lens together with a 20 µm pinhole and beam stop. An energy resolution of 2.0% at 16 keV has been achieved.     

An investigation of x‐ray escape for an HPGe detector

X‐ray escape peaks for a planar HPGe detector were investigated for a point source of photons with 59.5 keV energy. The effect of the solid angle for the incident photons on the escape probability of Ge K x‐rays was studied using collimators with varying apertures. A Monte Carlo program was also developed to estimate the probability of escape for various mechanisms and routes. The experimental and simulation results showed that the escape probability is essentially constant for a wide range of collimator radii, but at first starts to increase and then becomes constant when the side surface of the detector becomes accessible for escape with larger collimators. Copyright © 2003 John Wiley & Sons, Ltd.     

Background of x‐ray nanophotonics based on the planar air waveguide resonator

The work elucidates some model details of x‐ray flux waveguide resonance propagation through a planar, narrow, extended slit. The phenomenological substantiation of the correctness of the introduction of the waveguide resonance model is confirmed on the basis of the concept of flux spatial coherence. The peculiarities of the model realization in various designs of planar x‐ray waveguide resonators (PXWR) are discussed. The main fields of practical application of PXWRs are characterized by experimental results. Nanophotonics perspectives using waveguide resonance structures are outlined. Copyright © 2007 John Wiley & Sons, Ltd.     

Nanoresolution interface studies in thin films by synchrotron x‐ray diffraction and by using x‐ray waveguide structure

In the last years we performed several measurements with synchrotron radiation of several facilities to reveal interesting interface phenomena on the nanoscale. We used both x‐ray diffraction [1] , [2] (XRD) and spectrometry techniques. In this paper, we briefly summarize the results obtained from diffraction measurements, which lead us to our recent grazing incidence x‐ray fluorescence analysis (GIXRF) and extended x‐ray absorption fine structure (EXAFS) experiments. We show how a combination of experimental methods of GIXRF analysis and EXAFS spectroscopy in fluorescence detection with x‐ray standing waves (XSW) technique was applied for the depth profiling of a‐Si/Co/a‐Si layers with nanometer resolution to monitor the growth of CoSi intermetallic phase. The investigated layers were placed into the waveguide structure formed by two Ta films to increase sensitivity and accuracy of the measurements. Copyright © 2009 John Wiley & Sons, Ltd.     

A novel monochromator for experiments with ultrashort X‐ray pulses

Aiming at advancing storage‐ring‐based ultrafast X‐ray science, over the past few years many upgrades have been undertaken to continue improving beamline performance and photon flux at the Femtoslicing facility at BESSY II. In this article the particular design upgrade of one of the key optical components, the zone‐plate monochromator (ZPM) beamline, is reported. The beamline is devoted to optical pump/soft X‐ray probe applications with 100 fs (FWHM) X‐ray pulses in the soft X‐ray range at variable polarization. A novel approach consisting of an array of nine off‐axis reflection zone plates is used for a gapless coverage of the spectral range between 410 and 1333 eV at a designed resolution of E/ΔE = 500 and a pulse elongation of only 30 fs. With the upgrade of the ZPM the following was achieved: a smaller focus, an improved spectral resolution and bandwidth as well as excellent long‐term stability. The beamline will enable a new class of ultrafast applications with variable optical excitation wavelength and variable polarization.     

High‐resolution x‐ray analysis with multilayer gratings

Periodic multilayers are nowadays widely used to perform x‐ray analysis in the soft x‐ray range (photon energy lower than 1 keV). However, they do not permit to obtain high‐resolution spectra such as natural or synthetic crystals. Thus, multilayers cannot resolve interferences between close x‐ray lines. It has been shown and demonstrated experimentally that patterning a grating profile within a multilayer structure leads to a diffractive optics with improved resolving power. We illustrate the use of an Mo/B₄C multilayer grating in the Fe L and C K spectral ranges, around 700 and 280 eV, respectively. First, in the Fe L range, the improved spectral resolution enables us to distinguish the Fe Lα and Lβ emissions (separated by 13 eV). In addition, using a sample made of a mix of LiF and an iron ore, we show that it is possible to easily resolve the F K and Fe L emissions. These examples demonstrate that an improved x‐ray analysis can be obtained with multilayer gratings when there is the need to study samples having elements giving rise to close emission lines. Second, in the C K range, by comparing C Kα spectra from B₄C and cellulose, we show that the shape of the emission band is sensitive to the chemical state of the carbon atom. Copyright © 2009 John Wiley & Sons, Ltd.     

Wavelength‐dispersive x‐ray fluorescence measurements on organic matrices: application to milk‐based products

A simple and fast method for the determination of a series of analytes (sodium, magnesium, phosphorus, sulfur, chlorine, potassium, calcium, iron, zinc) in milk‐based products by wavelength‐dispersive x‐ray fluorescence spectrometry was developed and validated. Reference values were obtained by inductively coupled plasma optical emission spectroscopy and by potentiometry for chloride. The investigated samples were commercial products obtained from various parts of the world. Pellets of 4 g were prepared under 2 t pressure. For each sample, three pellets were prepared and analysed. Limits of quantification and repeatabilities were evaluated for the described analytes. Calibrations were established with 29 samples and validation of the method was made using a second set of 29 samples. An evaluation of this alternative method was done by comparison with data from the reference methods, using robust statistics. Copyright © 2004 John Wiley & Sons, Ltd.     

A sagittally focusing double‐multilayer monochromator for ultrafast X‐ray imaging applications

The development of a sagittally focusing double‐multilayer monochromator is reported, which produces a spatially extended wide‐bandpass X‐ray beam from an intense synchrotron bending‐magnet source at the Advanced Photon Source, for ultrafast X‐ray radiography and tomography applications. This monochromator consists of two W/B₄C multilayers with a 25 Å period coated on Si single‐crystal substrates. The second multilayer is mounted on a sagittally focusing bender, which can dynamically change the bending radius of the multilayer in order to condense and focus the beam to various points along the beamline. With this new apparatus, it becomes possible to adjust the X‐ray beam size to best match the area detector size and the object size to facilitate more efficient data collection using ultrafast X‐ray radiography and tomography.     

Chemometrics and its applications to x‐ray spectrometry

Recent developments in curve fitting, multivariate calibration, and pattern recognition in chemometrics, and their application to x‐ray spectrometry, are reviewed. Relatively innovated algorithms, namely genetic algorithms, neural networks and support vector machines, are discussed. Together with the three algorithms, the performances of different algorithms are compared briefly, which mainly includes principal component analysis, partial least‐squares regression, factor analysis, cluster analysis, nearest neighbor methods, linear discriminant analysis, linear learning machine, and soft independent modeling of class analogy. In general, the chemometrics methods are superior to the conventional methods, such as Fourier transform and Marquardt–Levenberg algorithms, to a certain extent. Copyright © 2006 John Wiley & Sons, Ltd.