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In the presented study, X-ray photoelectron spectroscopy and total reflection X-ray photoelectron spectroscopy methods were applied to analyze the Ti (75 nm) and Pd (100 nm) nanolayers deposited on the Si substrate using magnetron sputtering. The aim of the research was to determine the elemental composition and surface homogeneity of the analyzed nanolayers before their irradiation with highly charged xenon ions and to estimate the detection limit of the X-ray photoelectron spectroscopy technique for various glancing angles. The measurements were conducted using the SPECS mono-XPS system in the Institute of Physics at the Jan Kochanowski University (Kielce, Poland). The experimental setup and measurement conditions for the studied Ti and Pd layers are described. The X-ray photoelectron spectroscopy spectra were registered both for the non-total (35° and 10° angles) and total reflection (2:2° for the Pd nanolayer and 1:5° for the Ti nanolayer) regimes. The position of the C 1s photoelectron peak was applied (C-C component, binding energy 284.8 eV) to calibrate energy. First, the homogeneity of the nanolayers was investigated. The analysis of spectra concentrated on investigating the photoelectron peaks and, consequently, on determining the following: the binding energy of electrons, the intensity and full width at half maximum of photoelectron peaks, the background level, and the elemental composition of the nanolayer surface. In this study, the detection limit of the X-ray photoelectron spectroscopy measurements for different photoelectron peaks was calculated in relation to the excitation angle. An improvement of the X-ray photoelectron spectroscopy detection limit by a factor of 3-6, depending on the type of photoelectron peak, was observed for the angles below the critical angle of the X-ray total reflection phenomenon. [ABSTRACT FROM AUTHOR]

In this paper, the low-angle X-ray spectroscopy and reflectometry techniques, namely: the total reflection X-ray fluorescence analysis, grazing emission X-ray fluorescence analysis, grazing incidence X-ray fluorescence analysis, X-ray reflectometry and total reflection X-ray photoelectron spectroscopy, are presented. These techniques are used in the scientific activity, in interdisciplinary applications, at the Institute of Physics of the Jan Kochanowski University in Kielce (UJK) and the Department of Physical Methods of the Holy Cross Cancer Center (SCO). The studies were conducted in international cooperation with the European Synchrotron Radiation Facility (ESRF, Grenoble, France), the University of Fribourg (Switzerland) and Elettra Sincrotrone Trieste (Elettra, Trieste, Italy). The physical basics of the techniques are discussed as well as experimental setups applying either X-ray tube radiation or synchrotron radiation. Examples of the study possibilities and interdisciplinary applications, presented in the article, include elemental content analysis in human biological materials, biological and environmental samples (total reflection X-ray fluorescence analysis) and depth profiling of silicon wafer impurities (grazing emission X-ray fluorescence analysis). The paper also presents depth profiling, morphology study and surface elemental and chemical composition analysis of titanium and titanium dioxides nanolayers deposited on different substrates and irradiated by Xe ions in high charge states (grazing incidence X-ray fluorescence analysis, X-ray reflectometry, total reflection X-ray photoelectron spectroscopy). [ABSTRACT FROM AUTHOR]

In this work synchrotron radiation based X-ray reflectometry method was applied for determination of morphology of TiO2 nanolayers, unmodified, and irradiated with low energy highly charged Xeq+ ions. Using the synchrotron radiation based X-ray reflectometry technique density, thickness, and roughness of the TiO2 nanolayers were determined. The results showed that the thicknesses of the nanolayers obtained with synchrotron radiation based X-ray reflectometry method agree within the experimental uncertainty with the declared thicknesses. Moreover, the density of the nanolayers is much lower than density of the bulk TiO2 due to their nanometer thickness. The results obtained for irradiated samples suggest possible amorphization and smoothening of the TiO2 nanolayers surface due to interactions of the highly charged ions. [ABSTRACT FROM AUTHOR]

Abstract X-ray diffraction (XRD), grazing incidence X-ray diffraction (GIXRD) and X-ray reflectometry (XRR) techniques were applied for analysis of titanium (Ti) and titanium (IV) oxide (TiO 2) nanolayers with thickness of 25 nm, 50 nm and 75 nm deposited on silicon, quartz and BK7 glass substrates. The aim of studies was investigating the crystal structure and morphology of the nanolayers in dependence on the substrate type. The chemical phases of nanolayers and substrates were determined by using the XRD and GIXRD measurements. The benefits of applying low angle GIXRD and XRR analytical techniques, both for substrate and nanofilm analysis, is discussed based on theoretical calculations and simulations. Additional, analytical capabilities of the XRR technique to nanolayer and substrate morphology analysis are presented. Simulated XRR curves for titanium (Ti) and titanium (IV) oxide nanolayers are discussed depending on the substrate type as well as the substrate and nanolayer roughnesses. Experimental reflectometry curves are presented for all titanium and titanium (IV) oxide nanolayers deposited on the different substrates. As the result of the XRR analysis, the nanolayer thickness and roughness together with substrate roughness are estimated. The mean values of the Ti and TiO 2 layer thickness and roughness are presented for all studied samples. The largest roughness, both for nanolayers and for substrates, is obtained for BK7 glass material. In the manuscript, sample properties, experimental setups and measurement conditions are presented in details. Highlights • Grazing incidence X-ray techniques used for analysis of Ti and TiO2 nanolayers. • Analysis of the grazing incidence X-ray diffractogram of the layers. • Analysis of the reflectometry curves and layer thickness and roughness estimation. • Discussion of the influence of the substrates on the nanolayers morphology. [ABSTRACT FROM AUTHOR]

The aim of this research is to develop a fast analytical method for multielemental analysis of the tobacco plant Virginia tobacco (cultivated in Poland) and tobacco products (cigarettes, cigars, cigarillos, snuff and two kinds of properly crafted tobacco such as a shisha and cigarette tobacco) distributed in Polish markets by means of a low-power benchtop total reflection X-ray fluorescence (TXRF) system. For this purpose, a set of certified tobacco materials and real samples was employed. In leaves and stalks of V. tobacco and tobacco products, a concentration of 18 elements (P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Br, Rb, Sr and Pb) was determined. Analyzing elemental composition of tobacco plants, one can see that concentrations of S, Ca, Ti, Mn, Zn, Sr and Pb are higher in leaves, whereas the concentrations of P, Cl, K, Fe Cu and Br are higher in stalks; the levels of Cr, Ni, As and Rb are comparable in both these parts of the tobacco plant. All of the parameters affecting sample preparation and TXRF measurements conditions were carefully evaluated. The accuracy and precision of the TXRF measurements were verified using an internal standardization approach for quantification. [ABSTRACT FROM AUTHOR]

Total reflection X-ray fluorescence analysis and X-ray powder diffraction were used for elemental and chemical composition analysis of 83 samples of human kidney stones. Samples came from patients after surgical removal of stones. Elements such as P, K, Ca, Fe, Zn, Ni, Br, Sr, and Pb were determined in all samples. Other elements Mg, S, Cl, Ti, V, Cr, Mn, Cu, Se, Rb, I, and Bi were found in some of the analyzed kidney stones (censoring effect). Descriptive statistics were calculated for all elements paying particular attention to the censored elements. From diffraction measurements, the following crystalline substances were determined in the stones: apatite, struvite, uric acid, weddellite, whewellite, magnesium phosphate, and calcium phosphate. Information of chemical composition was applied to classify the analyzed kidney stone into four groups. Statistical analysis of the results included multigroups comparison, testing of element concentration distribution, and elemental correlations in the dependence of kind of kidney stones. The presented studies are part of wider microbiological studies focusing on the correlation between different kinds of bacteria and fungi presented in the samples of kidney stones and their elemental as well as chemical composition. Information on stone composition can be helpful in understanding kidney stone formation and complemented by additional metabolic blood and urine tests. This, in turn, can lead to appropriate medical treatment together with the reduction of the risk as regards forming new stones. [ABSTRACT FROM AUTHOR]

Total reflection X-ray fluorescence (TXRF) analysis was applied in determination of low concentration of lead in samples of human biological materials. The determination of lead in human serum and hair samples is presented as an example. In serum samples, lead concentration was in the range from 0.013 to 0.051 μg/g (median 0.024 μg/g). The reference ranges of lead content in hair are from 1.41 to 4.08 μg/g for men and from 1.18 to 3.29 μg/g for women groups, respectively. Because of Pb concentration range close to the detection limit of the TXRF method, the measurement needed evaluation of the best analytical conditions. This paper presents the results of this evaluation, namely internal standard selection, measurement conditions, and quantitative calibration of the spectrometer. Finally, as a result of evaluation, the detection limit was found on the level 0.001 μg/g (water solution) and about 0.005 μg/g for human hair samples and 0.007 μg/g for serum samples. The obtained values reach nearly the physiological lead level. The presented results are of practical importance for lead concentration studies in human biological materials using the TXRF method. Copyright © 2016 John Wiley & Sons, Ltd. [ABSTRACT FROM AUTHOR]

X-ray reflectometry and spectroscopic ellipsometry methods were applied for determination of physical properties of gold nonolayers. The nanolayers were prepared by sputtering of gold on different substrates: borosilicate glass, polished crystalline quartz and crystalline silicon. With X-ray reflectometry technique roughness of the substrates and density, thickness and roughness of gold layers were determined. The results showed decrease in density of the gold layers due to their nanometer thickness and that roughness of the underlayer affects roughness of the gold layer. In addition, thicknesses of the gold layers measured with spectroscopic ellipsometry turned out to be in agreement, within the experimental uncertainty, with results of the X-ray reflectometry method. [ABSTRACT FROM AUTHOR]

• The archaeological application of spectroscopic techniques is presented. • The elemental composition of selected historical Polish coins were obtained. • ED-XRF (made in NCBJ) results were compared to commercial WD-XRF, SEM-EDX, XRD. • Good agreement between different analytical values were obtained. The ED-XRF (energy-dispersive X-ray fluorescence) compact system was used to analyze selected Polish historical coins. The compact X-ray tube developed in the National Centre for Nuclear Research (NCBJ) was used as an X-ray source in the system designed for the ED-XRF studies. The XRF spectra were recorded with the Amptek SDD spectrometer. The elemental compositions of the coins have been determined using above mentioned system and the results were compared to those obtained with WD-XRF method. Other techniques such as SEM-EDX and XRD were also included into this work for comparison. The experimental data show that the X-ray system with transmission type X-ray tube with silver anode operating at 50 kV/30 µA which was developed in NCBJ together with the Amptek SDD spectrometer is an effective tool for chemical composition analyze of historical coins and can be successfully used in archaeometry. [ABSTRACT FROM AUTHOR]

Deficiency or excess of elements could disrupt proper functioning of the human body and could lead to several disorders. Determination of their concentrations in different biological human fluids and tissues should become a routine practice in medical treatment. Therefore the knowledge about appropriate element concentrations in human organism is required. The purpose of this study was to determine the concentration of several elements (P, S, Cl, K, Ca, Cr, Fe, Cu, Zn, Se, Br, Rb, Pb) in human serum and to define the reference values of element concentration. Samples of serum were obtained from 105 normal presumably healthy volunteers (66 women aged between 15 and 78 years old; 39 men aged between 15 and 77 years old). Analysis has been done for the whole studied population and for subgroups by sex and age. It is probably first so a wide study of elemental composition of serum performed in the case of Świętokrzyskie region. Total reflection X-ray fluorescence (TXRF) method was used to perform the elemental analysis. Spectrometer S2 Picofox (Bruker AXS Microanalysis GmbH) was used to identify and measure elemental composition of serum samples. Finally, 1st and 3rd quartiles were accepted as minimum and maximum values of concentration reference range. [ABSTRACT FROM AUTHOR]