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[en] In recent years, knowledge of the different chemical forms of the elements has gained increasing importance. There has been significant progress in methods that hyphenate chromatographic separations with atomic spectrometry. These hyphenated methods can provide the most complete information on the species distribution and even structure. However, they can be lengthy, relatively costly and difficult to bring to the routine. On the other hand, it is important to remember that chromatographic techniques represent only a minor part of the separation procedures available and, in certain cases, the application of basic chemistry to sample treatments can give quantitative information about specific chemical forms. In this sense, non-chromatographic procedures can provide methods that offer sufficient information on the elemental speciation for a series of situations. Moreover, these non-chromatographic strategies can be less time consuming, more cost effective and available, and present competitive limits of detection. Thus, non-chromatographic speciation analysis continues to be a promising research area and has been applied to the development of several methodologies that facilitate this type of analytical approach. In view of their importance, the present work overviews and discusses different non-chromatographic methods as alternatives for the speciation analysis of clinical, environmental and food samples using atomic spectrometry for detection.
[en] The application of a sufficiently high negative substrate bias, during the growth of tetrahedral amorphous carbon (ta-C), is usually associated with low sp3 bonding configuration and stressed films. However, in an effort to understand and utilize the higher pseudo thermo dynamical conditions during the film growth, at high negative substrate bias (- 300 V), reported here is a study on ta-C films grown under different hydrogen and nitrogen concentration. As grown ta-C films were studied under different negative substrate bias conditions. The variation of the sp3 content and sp3/sp2 ratio in the ta-C films exhibits a trend similar to those reported in literature, with a subtle variation in this report being the substrate bias voltage, which was observed to be around - 200 V, for obtaining the highest sp3 (80%) bonding and sp3/sp2 (3.95) ratio. The hydrogen and nitrogen incorporated ta-C films studied, at a bias of - 300 V, show an increase in sp3 (87-91%) bonding and sp3/sp2 (7-10) ratio in the range of studies reported. The inference is drawn on the basis of the set of data obtained from measurements carried out using X-ray photoelectron spectroscopy, X-ray induced Auger electron spectroscopy and Raman spectroscopy of as grown and hydrogen and nitrogen incorporated ta-C films deposited using an S bend filtered cathodic vacuum arc system. The study indicates the possibility of further tailoring ta-C film properties and also extending capabilities of the cathodic arc system for developing carbon based films for electronics and tribological applications
[en] X-ray photoelectron spectroscopy (XPS), also called electron spectroscopy for chemical analysis (ESCA), is widely used both in basic research and in analysis of materials, particularly in surface analysis. Using XPS we can obtain information on the elemental surface composition (except for H and He), and the electronic structure of the materials involved. This paper will briefly review the principle of XPS, basic qualitative and quantitative data analysis methods, and some application examples. (authors)
[en] Photoemission spectroscopy (PES) has been used widely to study the electronic structure of valence and core levels. However, conventional PES is surface-sensitive. To probe the interface and bulk properties of materials, hard X-ray photoemission spectroscopy (HXPES) has received increasing interest in the last decade, because of the deep probing ability of photoelectrons with higher kinetic energies (2-10 keV). Recently, a HXPES system was developed at the Canadian Light Source, using the high-energy version of a R4000 electron analyzer-based spectrometer connected to a medium-energy beamline, the soft X-ray microcharacterization beamline (SXRMB). Excellent performance of the beamline and the spectrometer is demonstrated herein using Au Fermi and 4f core lines; and the controlled probing depth of HXPES at SXRMB is demonstrated by tuning the photon energy (2-9 keV) in the study of a series of SiO2/SiC multilayer samples. Combined with the high-resolution X-ray absorption spectroscopy available at the SXRMB, the HXPES offers a powerful nondestructive technique for studying bulk properties of various materials. (author)
[en] Resistance switching phenomena in an amorphous Ni-Ti-O film were investigated. Very clear bipolar resistive switching characteristics were observed with good reproducibility. Stable retention and on/off pulse switching operation was demonstrated. An analysis of x-ray photoelectron spectroscopy of the Ni-Ti-O film provided a clue that the observed unusual bipolar resistance switching in the film is due to a microscopic change in the Ni-O and Ti-O binding states at the Ni-Ti-O film/electrode interface.
[en] Highlights: • The need by industry for small area analysis spurred the advent of the XPS Microprobe. • The Microprobe design allows for rapid x-ray induced secondary electron imaging. • Small areas of interest can quickly be located and analyzed. • Industrial applications include varied types of failure and contamination analyses. • Multipoint depth profiles can be obtained in one acquisition with one sputter crater. - Abstract: We will review the evolution of x-ray photoelectron spectroscopy (XPS / ESCA) instrumentation and applications that led to the development of the scanning XPS microprobe, describe its unique capabilities, and how they have impacted the use of XPS for industrial applications.
[en] In this study, the effects of corona plasma process on the dyeability and certain physical properties of woolen fabric were investigated. For this purpose, acid and 1.2 metal complex dyes, which are the most applicable dyes in the wool market were used. The patterns were examined to assess their dyeability, wettability, pilling resistance, alkali solubility, and strength values. The surface morphology and chemical structures were tested by X-ray photoelectron spectroscopy and alkali solubility analyses and also scanned by electron microscopy. Hydrophility indexes of the dyes that were used were determined. With the results of the experiments, their hydrophobic index is of vital importance, which is a factor for plasma efficiency on color depth. By using plasma treatment on woolen fabric, it is achievable to get a product with high hydrophility and pilling resistance values, dyeability, and less burdened dyeing bath.
[en] XAFS and X-ray Photoelectron Spectroscopy (XPS) are element specific techniques used in a great variety of research fields. The near edge regime of XAFS provides information on the unoccupied electronic states of a system. For the detailed interpretation of the XAFS results, input from XPS is crucial. The combination of the two techniques is also the basis for the so called core-hole clock technique. One of the important aspects of photoelectron spectroscopy is its chemical sensitivity and that one can obtain detailed information about the composition of a sample. We have for a series of carbon based model molecules carefully investigated the relationship between core level photoelectron intensities and stoichiometry. We find strong EXAFS-like modulations of the core ionization cross sections as function of photon energy and that the intensities at high photon energies converge towards values that do not correspond to the stoichiometric ratios. The photoelectron intensities are dependent on the local molecular structure around the ionized atoms. These effects are well described by molecular calculations using multiple scattering theory and by considering the effects due to monopole shake-up and shake-off as well as to intramolecular inelastic scattering processes.
[en] Complete text of publication follows. Nanotechnology has a high potential to engineer and alter basic properties of materials, and to exploit unusual phenomena observed on the nanometer scale. Consequently, the development of nanomaterials is already involved in a vast range of application fields, however, most of their characteristics are still underexamined, and relevance of studies on their environmental fate, toxic effects and other health risks have just been recognized. Besides, environmental effects and high costs of present production technologies definitely outline a need of both competitive and eco-friendly alternatives. It is well known that microbial production of nanoparticles may offer new perspectives in the field of bionanotechnology since it provides clean, inexpensive and 'green chemistry' techniques, which are especially desired in the future when technology transfer to large-scale production is concerned. In the last years the development of biosynthetic methods was an exponentially growing field, which focused on nanoparticles of noble metals, elemental and composite semiconductors with diameters in the range of 5-100 nm. We initiated the set-up of a new laboratory for studying biosynthesis processes of nanoparticles. The primary goal of this project is to realize the ability of controlling the size of nanoparticles by the conditions of the synthesis, which is motivated by the fact that the optoelectronic and chemical properties are sensitively dependent on this single parameter in addition to their elemental composition. In general, the characterization of nanoparticles, as well as measurements of structural properties require the presence of dedicated analytical infrastructure. The local availability of techniques like TEM, SEM, EDX, XPS, EELS, SIMS/SNMS, AFS, ICP-MS and spectrophotometry provides an advantageous background to consolidate bionanotechnological programs in our institute. As a result of our first test experiments selenium nanoparticles were successfully synthesized by non-pathogenic Lactobacillus strains. Batch cultures were incubated at 37 degC in MRS nutrient medium supplemented with 0.5 mM Se(IV) solution. Selenite oxyanions functioned as terminal electron acceptors in anaerobic respiration, which lead to the formation of elemental Se(0) nanospheres with a diameter of 150-250 nm as measured in SEM images (Fig. 1). The elemental analysis of the observed nanospheres was also performed, which is shown in Fig. 2.
[en] Highlights: • Optimal tuning parameters for three parameter choice methods were sought. • Two profile shapes and three regularization orders were used. • Compromise tuning parameter values for 1st order regularization are suggested. - Abstract: Composition depth profiles were extracted from simulated ARXPS data using regularization, with the regularization parameter determined by three different methods (Robust GCV, Modified GCV, and the Discrepancy Principle) that require tuning parameters. For each method, the optimal tuning parameter was determined for two input profile shapes, three Tikhonov regulators (0th, 1st, and 2nd order), and data noise ranging from 1% to 9%. Although universally applicable optimal tuning parameters were not identified, it was found that certain values could consistently produce acceptable results for the input profiles used in this study