Energy Dispersive X-ray Fluorescence Spectrometer Research Articles

Differences in the force system delivered by different beta-titanium wires in elaborate designs.

Objective: Evaluation of the force system produced by four brands of b-Ti wires bent into an elaborate design. Methods: A total of 40 T-loop springs (TLS) hand-bent from 0.017 x 0.025-in b-Ti were randomly divided into four groups according to wire brand: TMATM(G1), BETA FLEXYTM (G2), BETA III WIRETM (G3) and BETA CNATM (G4). Forces and moments were recorded by a moment transducer, coupled to a digital extensometer indicator adapted to a testing machine, every 0.5 mm of deactivation from 5 mm of the initial activation. The moment-to-force (MF) ratio, the overlapping of the vertical extensions of the TLSs and the load-deflection (LD) ratio were also calculated. To complement the results, the Young's module (YM) of each wire was determined by the slope of the load-deflection graph of a tensile test. The surface chemical composition was also evaluated by an energy dispersive X-ray fluorescence spectrometer. Results: All groups, except for G2, produced similar force levels initially. G3 produced the highest LD rates and G1 and G4 had similar amounts of overlap of the vertical extensions of the TLSs in "neutral position". G1 and G3 delivered the highest levels of moments, and G2 and G3 produced the highest MF ratios. b-Ti wires from G3 produced the highest YM and all groups showed similar composition, except for G2. Conclusion: The four beta-titanium wires analyzed produced different force systems when used in a more elaborate design due to the fact that each wire responds differently to bends.

Preparation of nano-titanium dioxide from ilmenite using sulfuric acid-decomposition by liquid phase method

In this study, high purity nano-TiO2 was prepared from Panzhihua ilmenite using sulfuric acid-decomposition by liquid phase method. The effects of H2SO4 molar volume, reaction time, initial pre-heating temperature and H2SO4 concentration on the decomposition rate of ilmenite were investigated in detail. The results showed that the decomposition rate reached 95.21% under the optimal conditions. The resulting titanium solution was qualified with 121g/L Ti4+. Since the initial pH value of hydrolysis system was below 3, the precipitation of metatitanic acid was obtained by direct hydrolysis of the titanium solution. On the other hand, the well-crystallized anatase and rutile were achieved at different calcination temperatures. The purity of the as-prepared TiO2 was above 99% with an average particle size of about 40–100nm. The ilmenite ore, intermediates and final products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray fluorescence spectrometer (EDS), X-ray fluorescence spectroscopy (XRF), thermal gravimetric analysis (TG), inductive coupled plasma emission spectrometer (ICP) and spectrophotometer. The results demonstrated that the process was suitable for industrial production because it was inexpensive, environment-friendly and promising in the preparation of high purity nano-TiO2.

Quantitative analysis of precious metals in automotive shredder residue/combustion residue via EDX fluorescence spectrometry

The recovery of precious metals from automotive shredder residue (ASR) dust/combustion residue is an option that is not usually considered due to the lack of available information. Therefore, before any disposal or recovery application can be considered, it is necessary to determine the significance of the levels and distribution of precious metal in ASR dust/ASR combustion residue. In the present study, quantitative analysis of precious metals (Pt, Pd, Au, Ag and Cu) in the ASR residue samples was performed using energy dispersive X-ray (EDX) fluorescence spectrometer. With the fundamental parameter (FP) method, the X-ray intensity is obtained and the quantitative analysis is performed using theoretical calculation. This method is very effective for quantitative analysis of unknown samples without standard samples. Further, in order to analyse the precious metal distribution within the ASR combustion residues, the microstructural characterisation and elemental mapping were also carried out with the aid of field emission scanning election microscopy combined with electron dispersive spectroscopy (FE-SEM EDS). Significant amount of Pt, Pd, Au, Ag and Cu element concentrations in the ASR residue were identified. Total precious (Pt, Pd, Au, Ag and Cu) metals obtainable values are representing about 12.23 wt% from its initial ASR dust/combustion residues. Considering their relevant concentrations, these metals should be properly recovered for recycling purposes before to dispose or landfill.

The native development of ancient Chinese glassmaking: a case study on some early lead-barium-silicate glasses using a portable XRF spectrometer

In this paper, a portable energy-dispersive X-ray fluorescence spectrometer was used for the nondestructive analysis of 41 lead–barium–silicate glass artifacts dated from the Warring States Period to the Han Dynasties (475 BC–220 AD). These glasses mainly are ornament, funeral and ritual vessels unearthed from different provinces of China. Based on the chemical compositions obtained, the affects of surface weathering on the quantitative results, the characteristics of chemical compositions and the colorants were discussed. Meanwhile, referred to the research results reported and historical background, the raw materials, the distribution, the cause, the origin and the production center of the lead barium glass were also discussed. The present research provides new valuable information for tracing the origin and transfer of glassmaking techniques of ancient China. Copyright © 2015 John Wiley & Sons, Ltd.

Effects of Bleaching Agents Combined with Regular and Whitening Toothpastes on Surface Roughness and Mineral Content of Enamel.

The purpose of this study was to evaluate surface roughness and changes in the composition of enamel submitted to different bleaching protocols and toothbrushing with regular and whitening toothpastes. Bleaching treatment could promote morphological and chemical changes in enamel surface. Enamel blocks were randomized into nine groups (n=10) according to the bleaching treatment (no bleaching, control group; 6% hydrogen peroxide, HP; or 10% carbamide peroxide, CP) and toothpaste used (placebo, PL; regular, R; or whitening dentifrice, W). Bleaching was performed according to manufacturers' instructions and all groups were submitted to 30,000 cycles of simulated toothbrushing with toothpaste (PL, R, or W). Mineral content evaluation and enamel roughness were evaluated initially (T1), after bleaching (T2), and after toothbrushing (T3), using an energy-dispersive micro X-ray fluorescence spectrometer and profilometry, respectively. Data were statistically analyzed with two way ANOVA, Tukey, and Dunnett tests (5%). Enamel surface roughness was influenced by bleaching and toothbrushing. Surface roughness increased for the groups that brushed with the placebo dentifrice (CP+PL, HP+PL, C+PL) and for the control group that brushed with whitening dentifrice (C+W). Enamel Ca/P ratio decreased after bleaching, but toothbrushing, regardless of the dentifrice used, did not reduce the enamel mineral content. The bleaching treatment resulted in a decrease of enamel mineral content, but the studied dentifrices did not contribute to surface mineral loss.

Major Oxides and Trace Elements Composition of Phosphate Bearing Sedimentary Rocks from Sokoto, Northwest Nigeria

Major and trace elements composition of phosphate rocks from phosphate bearing areas of Sokoto basin north-western Nigeria were investigated using PANanalytical Minipal4 PW4025/45B energy dispersive x-ray fluorescence spectrometer (EDXRF). The results indicated that CaO, P2O5 and SiO2 with mean concentration values ranging from 45.1±1.5 to 51.3±1.9 %, 19.9±1.0 to 21.6±2.2 % and 5.0±0.7 to 7.6±1.7 % respectively, are the most abundant species in Sokoto phosphate rocks (SPRs). Average concentrations of alkali metals were found to be less than 1wt % showing that very little salt will be added to agricultural soils via direct application of SPRs. The low concentration values recorded for alkali metals confirms the effectiveness of SPRs as good source of soil phosphorus. The estimated mean reactivity values varies from 2.2 to 2.4. These values underscore the suitability of SPRs as good raw material for fertilizer production. Cr, V, Cu and other studied trace elements were found to be enriched in the studied samples. Hence, direct application of SPRs can compete favourably with the conventional chemical fertilizers in enhancing the availability of soil nutrients for plant growth.

Source Identification of Volatile Organic Compounds and Particulate Matters in an Urban and Industrial Areas of Turkey

Elevated levels of volatile organic compounds (VOCs) and particulate matters have been observed in recent years in Kocaeli, Turkey, despite improvements in pollution prevention technology that have led to a reduction in gas and particulate emissions. Local authorities should devise alternative strategies to reduce the possible health effects of a variety of pollutants that affect air quality. The objective of this study was to identify potential sources of VOCs, fine particulate matter (PM2.5) and coarse particulate matter (PM10) concentrations in atmospheric aerosols that were collected in the highly industrialised area of Kocaeli, Turkey, during the winter and summer months by using wind directions. Samples were collected from May 2006 to January 2007, and concentrations of eight elements (As, Cr, Cu, Mn, Ni, Pb, V and Zn) were measured using energy dispersive X-ray fluorescence (EDXRF) and wavelength dispersive X-ray fluorescence (WDXRF) spectrometer. Samples were analysed for thirteen VOCs, including benzene, toluene, m/p-xylene, o-xylene, ethylbenzene, styrene, cyclohexane, 1,2,3-trimethylbenzene, 1,2,4trimethylbenzene, hexane, nonane and dodecane using thermal desorption (TD) and a gas chromatography/flame ionisation detector (GC/FID). The results show that vehicular emissions, oil and coal combustions, petroleum refinery and hazardous and medical waste incinerator are the significant sources of VOCs, PM 2.5 and PM 10 concentrations in Kocaeli.

Application of X-ray Fluorescence Spectrometers for Biopharmaceutical Forensics

In biopharmaceutical drug development and production, a portable energy dispersive x-ray fluorescence (EDXRF) spectrometer can be used for identification of foreign particles, investigation of discolored solutions, and improvement of process understanding. The spectrometer is a safe, small, robust, rapid, easy-to-use, multielemental diagnostic tool. Examples using the EDXRF for detecting metal composition in particulates, precipitants, liquids, and resins-with rapid resolution of investigations-are described.

Element Analysis Based on Energy-Dispersive X-Ray Fluorescence

Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a nondestructive, rapid, multielement, highly accurate, and environment friendly analysis compared with other elemental detection methods. Thus, EDXRF spectrometry is applicable for production quality control, ecological environment monitoring, geological surveying, food inspection, and heritage analysis, among others. A hardware platform for the EDXRF spectrometer is designed in this study based on the theoretical analysis of energy-dispersive X-ray. The platform includes a power supply subsystem, an optical subsystem, a control subsystem, and a personal computer. A fluorescence spectrum analytical method is then developed to obtain the category and content of elements in a sample. This method includes qualitative and quantitative analyses. Finally, a series of experiments is performed. Results show that the precision of the proposed measurement method is below 8%, whereas its repeatability is below 2%.

Pulsed bias effect on crystallinity and nano-roughness of Ti6Al4V-N films deposited by grid assisted magnetron sputtering system

This paper reports the effect of pulsed bias in comparison with DC bias on reactive deposition of Ti6Al4V-N films, obtained by Grid Assisted Magnetron Sputtering. The results obtained by X-Ray diffraction (XRD), Energy Dispersive X-ray Fluorescence Spectrometer (EDX) and Atomic Force Microscopy (AFM) show that bias condition affects the crystalline texture and change the roughness and morphology of the films. The DC bias favors the film crystallinity, however the pulsed bias produces smoother films.

Calibration for ED-XRF profiling of coal cores for the Itrax Core Scanner

Recent developments in instrumentation mean that chemical analysis of large drill cores taken for geological purposes can be performed rapidly at sub-millimetre scales using core scanners equipped with energy-dispersive X-ray fluorescence spectrometers. The present study describes the development of a calibration for the Itrax Core Scanner (Cox Analytical, Sweden), intended for whole cores of coal-seam sections, without the need for sample preparation. The calibration was developed for key major elements (Al, Si, P, S, K, Ca, Ti, and Fe) based on pressed pellets of reference coals, allowing semi-quantitative and, at times, quantitative analyses. The influence of core curvature and surface roughness compared with an ideal flat-surface was also examined using model samples, and their influence on the apparent sample composition evaluated.

Trace and major metal abundances in the shale and coal of various seams at Okaba coal mine, Kogi State, Nigeria

The distribution of a number of trace and major elements in the shale and coal of differing seams in Okaba, Kogi State, Nigeria, was studied using energy dispersive x-ray fluorescence spectrometer. The study was necessary to compare the quality of Okaba coal to world standards of coal quality. Major elements of Al, K, Ca and Fe showed concentration ranges of 5.93±2.49 – 8.42±0.003 mg/g, 0.18±0.46 – 2.16±0.0 mg/g, 0.53±0.41 – 2.23±0.35 mg/g and 6.05±0.004 – 18.28±1.2 mg/g respectively. The mean concentrations are 7.24mg/g (Al), 1.25 mg/g (K), 0.91 mg/g (Ca) and 11.86 mg/g (Fe). These values are clearly above the recommended concentrations in coal quality standards and for air emission standards by the World health organization. Trace metals of Ti, Cr, Mn, V, Ni and Cu showed concentration range of 0.84±0.007 – 2.98±0.007 mg/g , 0.03±0.0 – 0.12±0.025 mg/g, 0.02±0.11 – 0.30±0.02 mg/g, 0.02±0.44 – 0.2±0.05 mg/g, 0.01±0.075 – 0.12±0.001 mg/g and 0.03±0.02 – 0.62±0.001 mg/g respectively. These results indicate that Okaba coal and shale is enriched in the major elements analysed in comparison to worldwide averages of coal while the trace elements with exception of Ti are below the coal quality standards. Correlations between the various metals were also established. The S content correlated inversely well with the K content of both the shale and coal. Expectedly, the percentage Si content was high in the shale1 (26.70%) and shale2 (26.38%), while the lowest concentration was recorded at Okaba coal seam 5 (6.58%). The absence of Cl, Br, Na, and Mg in the samples clearly indicates the extent of surface leaching on the study area. This is evident by the various mountainous depressions in the study area. Keywords : Trace metals, EDXRF, coal, shale, major metals, seam.

In vivo EDXRF scanning analysis of human nail

This paper presents the results of a new technique for in vivo energy dispersive X‐ray fluorescence (EDXRF) scan analysis, applied to human fingernails. The scan employs a specially designed EDXRF spectrometer, which allows a concentration profile of the elements detected in a human nail. In order to carry out this technique, a group of nail fragments taken from different people was analyzed. The elements S, Ca, Cu, Fe, Cu, Zn, and Pb were detected in most of the samples. A bidimensional (x, y) scan was also performed on a whole removed nail in which the 2D spatial distribution of the detected elements was observed. Significant differences in some of the detected elements were noted. Minimum time of average detection per element was determined, based on the EDXRF spectra of the nail fragment. The time required to obtain an in vivo element profile of a typical nail was thus determined, applying the same geometry and acquisition conditions for all cases. The dose that the person undergoing this type of EDXRF scan analysis would be exposed to was also determined. Exposure time does not exceed 15 s, and the calculated administered dose is in the surface nail region of 0.1 mGy/s. The results of this study demonstrate that it is possible to carry out an in vivo X‐ray fluorescence scan analysis. This information may be used in different fields of medicine, such as nutrition and toxicology, and in other areas that establish a correlation between the concentration of the detected elements and certain diseases. Nail and hair are known to be ‘accumulating tissues’ unlike bodily fluids. In some aspects, nail analysis can be equal to a blood test. Copyright © 2014 John Wiley & Sons, Ltd.

A Rapid Determination Method of <sup>40</sup>K Concentration in the Soil

The pressed powder sample was determined by Epsilon 5 high-energy polarized energy dispersive X-ray fluorescence (EDXRF) spectrometer. The correlation coefficient of the standard curve method is 0.991 0. The precision is 2.98% and the relative deviation of the measurement standard samples is up to 6.40%, which showed that the precision and accuracy of the method were also good. Simultaneous measurement of seven soil samples with this method and γ-spectrometer were carried, the results of two analytical methods was compared using a paired t-test by SPSS program, which showed that there was no significant difference in the two sets of data. The results predicated that EDXRF could be a potential simple method for analyzing 40K in soil samples.

The Photon Attenuation Coefficients of Building Materials Containing with Lead Carbonate (PbCO<sub>3</sub>)

The total mass attenuation coefficient (μ/ρ, cm2 g-1) of gamma-ray for building materials containing with Lead Carbonate (PbCO3) have been studied. The raw building material have cement, sand and stone in the ratio 1 : 2 : 4. The raw material was mixed with 30% of PbCO3 to be used as the sample material. The mass attenuation coefficient of the raw material has been calculated by theoretical approach using WinXCom program for the photon energy band from 1 keV to 100 GeV. The composition of sample material was analyzed by energy dispersive X-ray fluorescence spectrometer (EDXRF). The variations of mass attenuation coefficient are shown graphically and compared with that of standard shielding concretes. It was found that the sample building material has higher value of mass attenuation coefficient than standard shielding concretes at energy zone above 2–7 keV, 90–800 keV and 5 MeV–100 GeV.

Aerosol filter analysis using polarized optics EDXRF with thin-film FP method

Interest in atmospheric aerosol issues has been increasing worldwide. X-ray fluorescence (XRF) is an important atmospheric aerosol monitoring tool for inorganic component analysis, because XRF is a rapid and easy analysis method. In particular, Energy dispersive X-ray fluorescence (EDXRF) has drawn attention for aerosol analysis. However, EDXRF has difficulties that: (1) many overlapping peaks exist for aerosol filter analysis and (2) many thin-film standard samples are required when an empirical calibration method is employed. Accurate analysis method of aerosol filter samples without the need for large sets of standards by semi-quantitative analysis software RPF–SQX (Rigaku profile fitting–spectra quant X), which includes the exact profile fitting and thin-film fundamental parameter (FP) method, is described using the EDXRF spectrometer equipped with secondary targets and polarized optics.

Geology and Geochemistry of Zungeru Amphibolites, North Central Nigeria

Basement rocks of Zungeru area consist of gneisses, schists, migmatites and intercalations of amphibolites and quartzites .This work involves detailed geological and geochemical investigation of Zungeru amphibolites so as to reveal their possible protolith. Field investigations show two petrographic types of the amphibolites on the basis of their textures, structures and mineralogy. They include the banded and massive types. The banded type is medium grained, strongly foliated and dark coloured rock while the massive type is fine to medium grained, dark-grey to black coloured with very weak foliations. Both types have been fractured due to deformation resulting in the development of joints and faults. Twelve representative samples of the amphibolites in the study area were collected and analyzed for major and trace elements using the Energy Dispersive X-Ray Fluorescence (EDX-RF) Spectrometer, Model: Minipal 4 at the laboratory of the National Geological Agency, Kaduna. However, only the major elements data was used for determination of the protolith of the amphibolites. The analytical results show that the Zungeru amphibolites contain on average 50.15% SiO2,12% Al2O3, 0.39% Na2O, 0.02% K2O, 9.41% CaO, 9.90% MgO, 0.02% MnO, 12.24% Fe2O3, 4.89% FeO, 0.5% TiO2, 0.10% P2O5 and 0.78% H2O. Various bivariate plots indicate that the precursors of the amphibolites are sedimentary. They are inferred to have been formed from metamorphism of decarbonated mixtures of pelitic sediments and calcite or dolomite. The occurrence of the amphibolites in association with quartzites further strengthened the fact that their origin is sedimentary and therefore referred to as para-amphibolites. African (600 ma) granitic series commonly called older granite suites. The most pervasive tectonic fabric of igneous reactivation of this suite is attributed to Pan-African event. This Precambrian crystalline basement complex covers nearly 60% of land surface of Nigeria and extends to neighboring countries. The migmatite-gneiss complex makes up about 60% of surface area of Nigeria basement. These rocks recorded at least four major tectonic cycles of deformation, metamorphism and remobilization in the Liberian, Eburnean, Kibarian and Pan-Africa, thus, confirming Russ's view of age of determination from various part of the Nigeria basement. The migmatite-gneiss complex rocks are believed to be basement rocks in real sense.

Nondestructive Determination of Allergenic and Toxic Elements in Jewelry: a Comparison of Benchtop and Portable Energy Dispersive X-Ray Fluorescence Spectrometers

X-ray fluorescence (XRF) is a widespread technique for alloy characterization and nowadays portable instruments are becoming popular. The objective of this study was to analyze necklaces, earrings, bracelets, rings and piercings by portable and benchtop XRF equipments, in order to verify if the presented methodology allows characterization of these objects, determining whether they meet - or not - current legislations regarding the concentrations of metals. Also to compare the equipments and check the feasibility of field measurements with portable equipments in just 5 s of analysis. In total 117 pieces were analyzed, surpassing 450 measurements. Nickel and Pb were found over the established limit in several samples, even on those attested as Ni- and Pb-free. It was possible to verify contents of noble or allergenic metals, with adequate detectability, low deviation and good agreement between both equipments employed, without sample treatment steps and without residue generation.

The Mass Attenuation Coefficients, Electronic, Atomic, and Molecular Cross Sections, Effective Atomic Numbers, and Electron Densities for Compounds of Some Biomedically Important Elements at 59.5 keV

The mass attenuation coefficients for compounds of biomedically important some elements (Na, Mg, Al, Ca, and Fe) have been measured by using an extremely narrow collimated-beam transmission method in the energy 59.5 keV. Total electronic, atomic, and molecular cross sections, effective atomic numbers, and electron densities have been obtained by using these results. Gamma-rays of241Am passed through compounds have been detected by a high-resolution Si(Li) detector and by using energy dispersive X-ray fluorescence spectrometer (EDXRF). Obtained results have been compared with theoretically calculated values of WinXCom and FFAST. The relative difference between the experimental and theoretical values are −9.4% to +11.9% with WinXCom and −11.8% to +11.7% FFAST. Results have been presented and discussed in this paper.

Heavy metal content of soil in urban parks of Belgrade

This study focuses on soil pollution in four urban parks of Belgrade. The sampling locations within each park were chosen based on proximity to streets characterized by heavy traffic, and soil samples were taken at different depths down to 50 cm. Concentrations of six heavy metals (Cr, Cu, Fe, Mn, Ni and Zn) were measured using Energy Dispersive X-Ray Fluorescence (EDXRF) spectrometer. The following average abundance order of heavy metals was found: Fe >> Mn > Zn > Cr > Ni > Cu in topsoil samples. The highest enrichment in topsoil was observed for Zn. Copper and Zn, metals mainly related to traffic emissions, exhibited the highest concentrations at the sampling location close to a bus and trolleybus terminus. The highest Ni and Cr concentrations were observed in a park located in a city suburb, where a large number of individual heating units is present. The largest decrease in concentrations with soil dept was observed for Zn and Cu, followed by Ni and Cr, in the parks with the highest concentrations of these elements in topsoil. Generally high topsoil Cr and Ni concentrations were observed in comparison with average values reported in literature for other world cities.