Determination of the Composition and Thickness of Co–Ni/Cr System Films by X-Ray Fluorescence

A procedure of determining the composition and thickness of Co–Ni/Cr two-layer films on Polycor by means of x-ray fluorescence is developed. The correction factors that take into account the effects of the mutual influence of the elements in the given system are calculated. The density of the materials entering into the composition of the films is determined experimentally. The metrological characteristics of the procedure are established.     

Identification of Urinary Stone Components by X‐Ray Photoelectron Spectroscopy

Abstract

X‐ray photoelectron spectroscopy (XPS) has been used for the first time to study the composition of calcium oxalate (CaOxa) stones and uric acid stones. This technique allows for the identification and location of various inorganic and organic species at the same time. In CaOxa stones, there were less than 10% of phosphates. Sectional analyses of these stones indicated that the content of phosphorus in the stone center is higher than that in stone crust. In uric acid stones, CaOxa was rarely found. XPS is able to detect differences in chemical functionality. In uric acid stones, the binding energy (E _b) for nitrogen atoms were about 399.5 ± 0.2 eV, which are largely characteristic of organic nitrogens N (?3). In comparison, the E _b values of N (+5) in inorganic compounds are about 401 eV.     

Application of Synchrotron X‐Ray Microbeam Spectroscopy to the Determination of Metal Distribution and Speciation in Biological Tissues

Abstract

Resolving the distribution and speciation of metal(loid)s within biological environmental samples is essential for understanding bioavailability, trophic transfer, and environmental risk. We used synchrotron x‐ray microspectroscopy to analyze a range of samples that had been exposed to metal(loid) contamination. Microprobe x‐ray fluorescence elemental mapping (µSXRF) of decomposing rhizosphere microcosms consisting of Ni‐ and U‐contaminated soil planted with wheat (Triticum aestivum) showed the change in Ni and U distribution over a 27‐day period, with a progressive movement of U into decaying tissue. µSXRF maps showed the micrometer‐scale distribution of Ca, Mn, Fe, Ni, and U in roots of willow (Salix nigra L.) growing on a former radiological settling pond, with U located outside of the epidermis and Ni inside the cortex. X‐ray computed tomography (CMT) of woody tissue of this same affected willow showed that small points of high Ni fluorescence observed previously are actually a Ni‐rich substance contained within an individual xylem vessel. µSXRF and x‐ray absorption near‐edge spectroscopy (XANES) linked the elevated Se concentrations in sediments of a coal fly ash settling pond with oral deformities of bullfrog tadpoles (Rana catesbeiana). Se distribution was localized within the deformed mouthparts, and with an oxidation state of Se (?II) consistent with organo‐Se compounds, it suggests oral deformities are caused by incorporation of Se into proteins. The range of tissues analyzed in this study highlight the applicability of synchrotron X‐ray microspectroscopic techniques to biological tissues and the study of metal(loid) bioavailability.     

Synchrotron X‐Ray scattering of polymer nanocomposites

Because of the importance of probing molecular-scale chemical and physical structure of environmental samples in their natural and often hydrated state, synchrotron radiation has been a powerful tool for environmental scientists for decades. Thus, the crucial role that a highly coherent and high-brightness hard X-ray source such as the Advance Photon Source (APS) can play in addressing many of the outstanding questions in molecular environmental science (MES) was recognized even before “first light” at the facility. No single synchrotron-based technique or experimental approach can adequately address the tremendous temporal and spatial heterogeneities of the chemistry, physics, and biology of natural environmental samples. Thus, it is common at the APS that multiple X-ray techniques and experimental systems are employed to investigate environmental samples, often chosen for their ability to focus on solute species, plants, microbes, organics, interfacial species, or solids.     

A New Method of X—Ray Holographic Tomography

A new method of x-ray holographic tomography,called pre-amplified x-ray holographic tomography,is proposed to develop an x-ray three-dimensional microscopic imaging technique.In this method,the key component is a micro zone plate taken as an imaging element like an optic lens in x-ray field.Some advantages of the method are shown by a numerical example.The method may make it possible to obtain x-ray microscopic imaging of biological specimens at high resolution in three dimensions.     

Trace Analysis of Al on Silicon Surfaces by Ultra‐soft X‐Ray Emission Spectroscopy

It is shown that near normal incidence, low‐energy electron excitation of Al on silicon surfaces by ultra‐soft X‐Ray emission spectroscopy yielded limits of detectibility (LD) in the picogram region. This result on L band emission via electron excitation is fully competitive with photon excitation using K‐α lines via grazing incidence total reflection techniques (TXRF). Surprisingly, it was also found that normal incidence synchrotron photon excitation on the same sample yielded much higher values of LD than low‐energy electron excitation, undoubtedly due to the use of a poor transmission grating used in the entrance optics.     

Analysis of the Structure of Thin Films of Zn‐Porphyrins by the Kinetics of the Fluorescence Anisotropy

The structure of thin films of Zntetraoctylphenylporphyrin (ZnTOPP) obtained by the spinning method is investigated. The kinetics of the decay of the fluorescence anisotropy of the films is analyzed in the form of a sum of exponents and by simulating the orientation of ZnTOPP complexes on the substrate (quartz) surface with allowance for the processes of the electron excitation energy transfer. The ZnTOPP films have a lamellar structure where individual layers form ordered domains. Within a domain, linear nonintersecting stacks of molecules are formed. In each stack the planes of the molecules are collinear, oriented perpendicularly to the surface of the substrate base, and form an angle of 45° with the directing axis of a stack.     

Photodegradation Studies by Laser‐Induced Fluorescence of the Reaction Product of 1,2‐Indanedione And Glycine

Photodegradation of the reaction product of 1,2‐indanedione with glycine in methanol at room temperature has been studied using laser-induced fluorescence. Samples were liquid solution and developed fingerprints on papers. Continuous laser excitation of fresh solution of 1,2‐indanedione–glycine dissolved in methanol shows that the emission peak at 564 nm reached a quite stable low level after almost 1 hr of continuous excitation. For latent fingerprints on papers developed with 1,2‐indanedione dissolved in methanol solution, the luminescence peak decreases for the first week and reached a stable level for almost 2 weeks. A long‐term study is needed to reach a conclusion on the stability of the samples (liquid and developed fingerprints) at room temperature conditions.     

Investigation of the Melt‐Crystallization of Polypropylene by a Temperature Slope Method

Abstract

To investigate the in‐situ ordering process of isotactic polypropylene (iPP) from a melt state, a stationary growth front was prepared by the temperature slope crystallization (TSC) method. During the melt‐crystallization, iPP was crystallized into the α‐phase or β‐phase depending on the crystallizing conditions. The mechanism of the melt‐crystallization at the growth front was precisely observed by wide‐angle and small‐angle x‐ray scattering (WAXS and SAXS) using a strong synchrotron beam. In the TSC apparatus, the sample was crystallized in between a heater, controlled to 220°C, and a cooler, cooled by water to 25°C. We define the z‐axis parallel to the temperature gradient. A‐lamellae and B‐lamellae are also defined as those whose lamellar normal are perpendicular and parallel to the z‐axis, respectively. In a sample‐stop (SS) stage before the TSC, the original α‐phase lamellae became thicker, approaching to the melt‐solid boundary by annealing. The annealing process showed that the α‐phase B‐lamellae remained and the SAXS reflection was stronger on the meridian near the melt‐solid boundary in the SS stage. In the beginning of the TSC, the α‐phase B‐lamellae developed as a primary crystallization. During secondary crystallization under high supercooling, the SAXS cross pattern appeared showing that the α‐phase developed both A‐ and B‐lamellae. As the growth direction of A‐lamellae is parallel to the z‐axis, A‐lamellae grow faster than B‐lamellae. By the self‐epitaxial mechanism on the side surface of the A‐lamellae, the B‐lamellae grow on the base of the A‐lamellae. Following appearance of a spontaneous β‐nucleus, the β‐phase lamellae grew preferentially, excluding the α‐phase, and occupied the whole area of the sample. In this case also, A‐lamellae are advantageous to grow because of the growth direction parallel to the z‐axis. As a result, the SAXS β‐phase reflection appeared on the equator.     

Determination of the Refractive Index of Dielectrics by Means of Light‐Induced Diffraction Gratings

Consideration is given to the possibilities of measuring the refractive index n of dielectric samples by means of spontaneous gratings produced by an spolarized laser beam in a photosensitive thin film applied to a sample in vacuum. With the specific choice of the film thickness, the value of n is determined from diffraction measurements of the period of a spontaneous grating with the error n = ±0.002. The method allows measurement of n isotropic and anisotropic samples within the range 1.32.5 on plane and cylindrical surfaces with the area determined by the section of the laser beam that induces the spontaneous grating. Examples of measurements of n on plane surfaces of glasses, a LiNbO₃ crystal, and on the cylindrical surface of a ruby rod are presented.     

Calculation of the Mass of X（3872） by the Mandelstam Generalization of the Gell-Mann-Low Method

On the basis of assuming that the narrow state X（3872） is a molecule state consisting of D0 and D＊0, we apply the Mandelstam generalization of the Ge11-Mann-Low method to calculate the matrix element of quark current between the heavy meson states described by Bether-Salpeter wave function. In calculation of the matrix element of quark current the operator product expansion is used in order to include the nonperturbative contribution of the vacuum condensates. In this scheme we calculate the mass of X（3872）. We believe that this scheme is closer to QCD than the previous work.     

Determination of Thermal Conductivity of Liquids by a Multi-Point Laser Pump Method

As an advanced optical method, a multi-point pump method is presented for measurements of thermo-physical properties of liquids. Meanwhile, based on the laser-induced thermal grating method, a new theory model is presented and used to analyse the thermal effects caused by the multi-point laser pump, by which the thermal conductivity of liquids can be obtained. The results of some typical liquids, such as water, ethanol and acetone, are presented and are consistent with those of acknowledged values, demonstrating that the multi-point method is simple and useful for characterizing thermal properties of liquids.     

Determination of the Local Parameters of a Cascade‐Arc Plasma by the Profiles of the Lines in the Radiation Spectrum

The transverse distribution of the plasma temperature in the positive column of a d.c. cascade arc in argon at atmospheric pressure has been measured. The measurements have been carried out by the conventional method involving the determination of the emissivity of plasma as well as directly from the radiation spectrum of the arc without recourse to the Abelian inversion. A theoretical and model justification of the applicability of the second method is given. The results of the determination of the temperature profile in the observation direction by the width and shift of the ArI 425.9nm line selected for the diagnostics are presented. An analysis of the data obtained supports the possibility of determining the temperature of an inhomogeneous, optically thin plasma from the profiles of lines in the emission spectrum.     

Determination of Arsenic and Mercury in Chinese Medicinal Herbs by Atomic Fluorescence Spectrometry with Closed‐Vessel Microwave Digestion

Abstract

A simple method was developed for the determination of trace arsenic and mercury in Chinese medicinal herbs. The samples were digested in closed‐Teflon vessels in a microwave oven, and followed with hydride generation atomic fluorescence spectrometric measurements. The experimental conditions for the digestion were carefully optimized using an orthogonal design. The accuracy of the method was validated by recovery experiments, and the analytical results for arsenic in seven medicinal herbs (Codonopsis pilosula, Radix angelicae sinensis, Aconitum carmichaeli debx, crude aconite root, giant typhonium rhizome, Rhizoma typhonii, and Radix aconiti lateralis preparata) were found to agree well with those by inductively coupled plasma atomic emission spectrometry (ICP‐AES). The linear dynamic range of the calibration curve was in the range of 0.1–400 ng/mL for arsenic, and the correlation coefficient was better than 0.999. The limit of detection was 0.1 ng/mL for arsenic. For mercury, the determination was accomplished through mercury cold vapor generation in the same instrumental system. The linear dynamic range was 0.03–250 ng/mL, with a limit of detection of 0.03 ng/mL for mercury. This was a rapid, convenient, precise, and cost‐effective method.     

Heterogeneous Chemiluminescence of Crystal Phosphors on X‐Ray or UV Irradiation

Using a highvacuum assembly with molecular beams and setups with an implemented atom probe, we investigated atomic and molecular adsorption luminescence of the oxides CaOBi and MgO in O and O₂ beams and also radicalrecombination luminescence excited by H and O atoms in ZnS and in ZnS,CdS samples activated with silver, copper, and the rareearth element Tm. It is established that exposure to UV light and xray radiation of the CaOBi, MgO, and ZnSTm samples, where the mechanism of direct excitation of heterogeneous chemiluminescence (HCL) is realized, does not influence the characteristics of the heterogeneous chemiluminescence, whereas similar exposure of the ZnS,CdSCu,Al and ZnS,CdSAg samples and of selfactivated ZnS, in which the excitation of heterogeneous chemiluminescence is due to the ionization of the lattice, leads to an increase in the intensity of heterogeneous chemiluminescence up to five orders of magnitude. The mechanisms of the phenomenon are considered.     

X‐Ray Luminescence of Thin Oxide Films Containing Lead and Bismuth

We obtained thin films of the Bi₄Ge₃O₁₂, Bi₄Si₂O₁₂, PbWO₄, and Bi₂WO₆ scintillators and investigated their luminescence properties on xray excitation. We measured the xray luminescence spectra and established the linear character for the dependence of the luminescence intensity on the power of the dose of xray irradiation within the limits of up to 3·10^–3 A/kg. We investigated the radiation stability of the films obtained. The possibility of their application for detecting ionizing radiation is investigated. The films based on Bi₄Ge₃O₁₂ with an admixture of the Ge and Si or Mn activator of up to 1.5 mol.% are most suitable.     

Hydroxypropyl-β-Cyclodextrin Enhanced Determination for the Vitamin B<Subscript>12</Subscript> by Fluorescence Quenching Method

A novel fluorescence quenching method for the determination of Vitamin B₁₂(VB₁₂) had been developed. It was based on that the fluorescence intensity of erythrosine sodium(ES) could be enhanced by Hydroxypropyl-β-cyclodextrin(HP-β-CD) due to the formation of inclusion complex (HP-β-CD-ES), while the fluorescence intensity of HP-β-CD-ES was diminished after adding VB₁₂ into the system, and there was a linear relationship between the fluorescence quenching value of the system (ΔF) and the concentration of VB₁₂(c). The mechanism of the determination of VB₁₂was discussed. The results showed that under the optimal conditions, the linear range of calibration curve for the determination of VB₁₂ was 0.0∼2.1 × 10⁻⁵ mol/L, and the detection limit was 1.8×10⁻⁷ mol/ L. It could be satisfactorily applied to the determination of VB₁₂ in injections.     

Luminescence of GaN Layers Grown on GaAs Substrates by the Method of Radical‐Beam Epitaxy

We have investigated the properties of GaN films obtained by the method of radicalbeam gettering epitaxy. At room temperature the photoluminescence spectra display a weak peak at 3.37 eV, with the fundamental radiation band being located in the range 1.7–2.0 eV. At the temperature 4.2 K, the band with an energy of 3.47 eV is present. The donoracceptor transition with a maximum at 3.26 eV and its phonon repetition dominate in the spectrum. A wide yellow band with a maximum at 2.10 eV and a weak peak at 2.88 eV are also observed. It has been established by Auger electron spectroscopy that gallium and nitrogen are the basic elements that enter into the composition of the film. Xray structural investigations have shown that the films possess a hexagonal structure.     

Statistical Method for Determination of the Photopeak Area of Scintillation γ-Spectra

A comparatively unsophisticated analytical statistical method is developed for determination of the parameters of the peak of full absorption processing scintillation γ-spectra. The generasl beckground under the photopeak is linearly approximated and an accuracy estimation was done. The method is illustrated with several applciaitons of non-destructive γspectroscopic analysis of ¹³⁷Cs in soil samples. Concentrations of the order of severals pCi¹³⁷Cs are determined accurately enough at disturbing influence of the peak of full absorption of RaC(²¹¹Bi) and 610 KeV. The control data was processed by means of a “Minsk-22” computer under a convenient programme. The results correspond to those obtained according to the described method at a reliable estimation of accuracy.     

Fluorescence Quenching of UVITEX‐OB by Aniline in Alcohols and Alkanes

Fluorescence quenching of UVITEX‐OB [2,5‐thiophenediylbis(5‐tert‐butyl‐1,3‐benzoxazole)] by aniline in different polar and nonpolar solvents was examined at room temperature by steady‐state fluorescence measurements. Positive deviations from the nonlinear Stern–Volmer plots were observed in most of the solvents indicating the extent of quenching to be large. The quencher concentration dependence data were analyzed using ground‐state complex and sphere of action static quenching models in order to interpret the results. The magnitudes of the quenching rate parameters suggest that a sphere of action static quenching model is expected to describe the data most accurately. Also, the results are suggestive of both static and dynamic quenching processes being responsible for the observed positive deviation in the Stern–Volmer plot. Experimental results are described by an equation derived using the finite sink approximation model, which allows the evaluation of diffusion‐limited interaction and the estimation of encounter distance and mutual diffusion coefficient independently.