The knowledge of atomic fundamental parameters, such as the fluorescence yields with low uncertainties, is of decisive importance in elemental quantification involving X-ray fluorescence analysis techniques. However, especially for the low-Z elements, the available literature data are either of poor quality, of unknown or very large uncertainty, or both. For this reason, the K-shell fluorescence yield of carbon was determined in the PTB laboratory at the synchrotron radiation facility BESSY II. In addition, theoretical calculations of the same parameter were performed using the multiconfiguration Dirac-Fock method, including relativistic and quantum electrodynamics (QED) corrections. Both values obtained in this work are compared to the corresponding available literature data.

A TXRF round robin test using preselected micro- and nanoscaled samples has been performed and shows excellent results, demonstrating the strength and reliability of the TXRF method when decoupled from unfavorable sample preparations.

Efficient soft X-ray spectroscopy in the laboratory is still a challenging task. Here, we report on new toroidal multilayer optics designed and applied with the laser-produced plasma (LPP) source of the Berlin Laboratory for innovative X-ray technologies. The optics are described and characterized, and the application of the updated source to scanning-free grazing emission X-ray fluorescence is demonstrated on thermoelectric gold-doped copper oxide nanofilms. The comparison with synchrotron measurements allows estimating a flux on the sample of approximately 7.5 × 109 photons/s in the 1 keV range on a 100 µm × 100 µm spot, emphasizing the suitability of the updated LPP source for the application in photon hungry experiments.

Grazing-Incidence X-ray fluorescence (GIXRF) analysis, which is closely related to total-reflection XRF, is a very powerful technique for the in-depth analysis of many types of technologically relevant samples, e.g. nanoparticle depositions, shallow dopant profiles, thin layered samples or even well-ordered nanostructures. However, the GIXRF based determination of the depth-dependent information about the sample is usually based on a modeling of the experimental data. This requires profound knowledge of the geometrical parameters of the setup employed, especially the incident beam profile as well as the detector aperture parameters. Together they determine the incident angle dependent so-called effective solid angle of detection which must be known in order to model any experimental data set. In this work, we demonstrate how these instrumental parameters, which are typically not known with sufficient accuracy, can be determined using dedicated experiments with a well-known calibration sample. In addition, this paves the way for a full calibration of the setup, as also information about other parameters, e.g. the incident photon flux is gained. Here, we are using a commercially available instrument for this demonstration but the principle can also be applied for other GIXRF setups.

With the advent of both modern X-ray fluorescence (XRF) methods and improved analytical reliability requirements the demand for suitable reference samples has increased. Especially in nanotechnology with the very low areal mass depositions, quantification becomes considerably more difficult. However, the availability of suited reference samples is drastically lower than the demand. Physical vapor deposition techniques have been enhanced significantly in the last decade driven by the need for extremely precise film parameters in multilayer production. We have applied those techniques for the development of layer-like reference samples with mass depositions in the ng-range and well below for Ca, Cu, Pb, Mo, Pd, Pb, La, Fe and Ni. Numerous other elements would also be possible. Several types of reference samples were fabricated: multi-elemental layer and extremely low (sub-monolayer) samples for various applications in XRF and total-reflection XRF analysis. Those samples were characterized and compared at three different synchrotron radiation beamlines at the BESSY II electron storage ring employing the reference-free XRF approach based on physically calibrated instrumentation. In addition, the homogeneity of the multi-elemental coatings was checked at the P04 beamline at DESY. The measurements demonstrate the high precision achieved in the manufacturing process as well as the versatility of application fields for the presented reference samples.

An experimental method for the verification of the individually different energy dependencies of L(1)-, L(2)-, and L(3)- subshell photoionization cross sections is described. The results obtained for Pd and Mo are well in line with theory regarding both energy dependency and absolute values, and confirm the theoretically calculated cross sections by Scofield from the early 1970 s and, partially, more recent data by Trzhaskovskaya, Nefedov, and Yarzhemsky. The data also demonstrate the questionability of quantitative x-ray spectroscopical results based on the widely used fixed jump ratio approximated cross sections with energy independent ratios. The experiments are carried out by employing the radiometrically calibrated instrumentation of the Physikalisch-Technische Bundesanstalt at the electron storage ring BESSY II in Berlin; the obtained fluorescent intensities are thereby calibrated at an absolute level in reference to the International System of Units. Experimentally determined fixed fluorescence line ratios for each subshell are used for a reliable deconvolution of overlapping fluorescence lines. The relevant fundamental parameters of Mo and Pd are also determined experimentally in order to calculate the subshell photoionization cross sections independently of any database.

At the COMPASS experiment at CERN's SPS many physics channels containing neutral particles are studied. These particles are identified by two electromagnetic calorimeters covering different transfers regions. For certain physics the main signature is described by these neutral particles which requires a calorimetric trigger system. The method described here is fully based on the existing front end electronics and uses digital pulse shape analysis techniques. This approach allows to implement a flexible trigger system as well as to reduce cost by avoiding to produce new electronic components. The implementation of this new trigger as well as the performance measured during the 2009 run will be discussed.

Ultrathin nanocomposite films of nitrobenzene on silicon were analyzed by Infrared Spectroscopic Ellipsometry (IRSE), X-ray reflectivity (XRR) and X-ray standing waves (XSW) before and after evaporation of gold. Infrared Spectroscopic Ellipsometry measurements were performed for identification of adsorbates and for investigation of the molecular orientation. Results for film thickness were correlated with XRR measurements. Further, XSW measurements of elements incorporated in nitrobenzene (C, N, and O) were performed with soft X-rays. The combination of the different methods allowed to confirm a model for the electrochemically deposited nitrobenzene films before and after gold evaporation. The characterization by XRR and XSW scans using hard X-rays showed that gold had penetrated into the nitrobenzene film and thus changed density and optical properties of this layer significantly. A depth profile correlated to the electron density is deduced from the XRR measurements. This profile allows to localize—in vertical direction—gold islands within the composite film.

When a work-piece is bended or deformed, internal stress in the piece leads to a change of its lattice constants.Consequently, stress gradients in the sample lead to lattice constant gradients.In order to determine these gradients as a function of depth below the sample surface the standard Twin-Mirror Arrangement was modified.Small slits were used both at the primary beam side and at the diffracted beam side to define a small sample volume on the omega axis of the diffractometer.A sample movement through this volume delivers one-dimensional depth information which is needed for stress gradient analysis.In order to take advantage of deeper penetration depths we used, in addition to the common Cu Kα radiation, the Mo Kα and Ag Kα lines.A bended aluminium test sample was characterized in depth by XRD with different photon energies.It is shown that the presented technique is capable of measuring relative lattice constant changes ε (in the range of 0.1% -0.3%) in depth.The advantages of using different photon energies are discussed as well.

An approach to the chemical characterization and a study of the morphology of very fine fractions of nanoparticles on surfaces can be deduced from experiments using the grazing incidence X-ray Standing Waves (XSW) by means of Total Reflection X-ray Fluorescence (TXRF). Some theoretical aspects not considered until now for TXRF and XSW, e. g. the influence of coherence length of X-rays from different X-ray sources, the particle form, particle size and distribution, are presented and discussed. Results of numerical simulations of XSW-scans considering the modelling of particles are compared with the experimental data obtained from XSW experiments performed at a synchrotron radiation facility. Advantages and limitations of the applied techniques are discussed for the characterization of Au- and CdTe-nanoparticles.

A microfocus x-ray tube with multiple targets and an electron gun with a focal spot size of 10 microm in diameter has been developed. The electron gun contains a LaB(6) cathode and an Einzel lens. The x-ray tube can be operated at 50 W (50 kV, 1 mA) and has three targets, namely, Cr, W, and Rh on the anode that can be selected completely by moving the anode position. A focal spot size of 10 microm in diameter can be achieved at 0.5 mA current. As demonstration of the usability of a multiexcitation x-ray tube, the fluorescence x-rays have been measured using a powder specimen mixed of TiO(2), Co, and Zr of the same quantity. The differences of excitation efficiency have clearly appeared according to the change in excitation source. From the results discussed here, it can be expected that the presented x-ray tube will be a powerful tool in microx-ray fluorescence spectrometers and various x-ray instruments.

The COMPASS experiment (COmpact Muon Proton Apparatus for Structure and Spectroscopy) is a fixed target experiment located at the CERN Super Proton Synchrotron. The physics program is focused on the study of hadron structure and hadron spectroscopy with high intensity muon and hadron beams, up to 160 GeV/c for muons and 190 GeV/c for hadrons respectively. To allow the tracking of charged particles with very low and as well very high momentum, COMPASS comprises two magnetic spectrometer stages extending to a total length of 60 m. From the data acquisition point of view, about 200000 analog detector channels have to be read along the complete experiment. Depending on the detector signal characteristics and the number of channels, this task is realized by frontend electronics using either dedicated ASICs and/or sampling analog-to-digital (ADC) or time-to-digital (TDC) components. The sampling ADC based readout system of the COMPASS experiment comprises today over 127k channels equipped with the APV25 frontend ASIC and 5728 direct sampling channels. An important feature from the beginning was the combination of data transfer, clock and trigger distribution and configuration access within a standardized serial interface between the different ADC modules and the first stage of data concentrator modules. By choosing between a copper or fiber realization for this interface, either a low cost interconnect or a link with galvanic decoupling can be realized. The ongoing development of the sampling ADC electronics is focused on the migration toward the Advanced Telecom Computing Architecture (ATCA) crate standard, to overcome the backplane bandwidth limitations in VME systems. In addition, the ATCA standard provides better cooling and monitoring capabilities. To simplify the transition to ATCA, the MSADC module was already realized as a mezzanine card, which can be mounted on an ATCA based carrier card as well. In addition, the MSADC card fits also to the MicroTCA form factor, - - which allows to provide a handy building block for laboratory based data acquisition systems.

Doubly-curved crystals (DCCs) can be very useful devices to focus and monochromatize radiation from an X-ray tube or a synchrotron, especially for X-ray fluorescence analysis. However, production of a DCC is somewhat difficult. In this paper we will present some basic theory about DCC geometries, different ways of DCC production and methods to test the quality of the DCCs.

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Since 2004 ISAS operates a dipole beamline at the synchrotron radiation facility DELTA at Undversity of Dortmund. Synchrotron radiation is used at this beamline as an excellent excitation source for X-ray fluorescence spectrometry (XRF). Among others, the high brilliance of the synchrotron radiation in contrast to conventional X-ray tubes, the strong polarization of the synchrotron radiation and the low divergence of the electron beam can be applied to XRF offering several advantages for spectroscopy. These outstanding features encouraged us to develop and operate a synchrotron radiation induced X-ray micro fluorescence probe connected to a wavelength dispersive spectrometer (SR-WDXRF). A relevant characteristic of such a device, namely, good lateral resolution at high spectral resolution can be applied for single spot-, line-scan and area map analyses of a variety of objects. The instrumentation of the SR-WDXPF and the performed experiments will be presented. Main task is the detection of light elements by their fluorescence K-lines and the specification of element compounds.

X-ray standing wave spectroscopy at grazing incidence ( GI- XSW) is demonstrated to be a versatile method to characterize multilayer thin films and element distributions on a nanometre scale. In this work we present a measurement procedure and development of a computerized simulation tool to interpret measured intensities. Four different kinds of samples are investigated. First, thickness determination of a set of thin germanium layers on silicon ranging from 29 nm to 1 mm is presented, which demonstrates the wide dynamic range that is feasible and the limitations that occur. Second, analysis of a sample of gold clusters evaporated on an 80 nm polystyrene film on a silicon substrate is shown. Low contrast organic mono-, double or multilayers is the third kind of sample to be characterized by XSW. Finally, qualitative and quantitative characterization of a laser multilayer mirror utilizing XSW and a fast Fourier transform evaluation method are described. Measurement and simulation procedures for each kind of sample are outlined in this report as well as the possibilities and limits of this XSW method.