Mineralogy of the clay fraction of soils from the moray cusco archaeological site: a study by energy dispersive X-ray fluorescence, X-ray diffractometry and M?ssbauer spectroscopy

The purpose of this work is to report the advances in the elemental and structural characterization of the clay fraction of soils from the terraces of the Moray Archaeological site, located 38 km north of the city of Cusco, Cusco Region. One sample was collected from each of the twelve terraces of this site and its clay fraction was separated by sedimentation. Previously the pH of the raw samples was measured resulting that all of the samples were from alkaline to strongly alkaline. Energy dispersive X-ray fluorescence (EDXRF) was used for the elemental characterization, and X-ray diffractometry (XRD) and transmission Mössbauer spectroscopy (TMS), using the ?? 14.4 keV nuclear resonance transition in ⁵⁷Fe, were used for the structural characterization of the clays and clay minerals present in each sample. The EDXRF analyses of all the samples show the presence of relatively high concentrations of sulfur in some of the samples and relatively high concentrations of calcium in all of the samples, which may be related to the high alkalinity of the samples. By XRD it is observed the presence of quartz, calcite, gypsum, cronstedtite, 2:1 phyllosilicates, and iron oxides. The mineralogical analysis of Fe by TMS shows that it is present in the form of hematite and occupying Fe^2?+? and Fe^3?+? sites in phyllosilicates, cronstedtite, and other minerals not yet identified.     

Analysis of some elements in three Chrysolina (Coleoptera, Chrysomelidae) species by EDXRF spectrometry

In this investigation, the concentration levels of potassium, calcium, iron, nickel and cadmium for three Chrysolina species were measured in the region of Erzurum (Turkey) located at latitude 40°17′ north and longitude 41°17′ east. The concentrations measured by energy dispersive X-ray fluorescence (EDXRF) spectrometry were analysed. Photons of 59.5 keV and 5.9 keV emitted, respectively, by an annular ²⁴¹Am and ⁵⁵Fe radioactive source were used to excite the characteristic X-rays of various elements present in the insect samples. These results are presented and discussed in this paper.     

Analysis of tincal ore waste by energy dispersive X-ray fluorescence (EDXRF) Technique

Etibank Borax Plant is located in K?rka-Eski?ehir, Turkey. The borax waste from this plant was analyzed by means of energy dispersive X-ray fluorescence (EDXRF). The standard addition method was used for the determination of the concentration of Al, Fe, Zn, Sn, and Ba. The results are presented and discussed in this paper.     

Determination of cobalt marker in cow ruminal fluid by EDXRF and SRTXRF

This article describes a comparison of conventional energy‐dispersive X‐ray fluorescence (EDXRF) and synchrotron radiation total‐reflection X‐ray fluorescence (SRTXRF) for Co determination in ruminal fluid from Holstein cow. This element is used as marker for animal nutrition studies. For EDXRF, 200 µl of the sample were dried on 6.35 µm Mylar film at 60 °C. The excitation was carried out using an X‐ray tube with Mo target and Zr filter operated at 30 kV/20 mA. For SRTXRF, 10 µl of the sample were pipetted on a Lucite carrier and dried at 60 °C. In both the techniques, Ga was used as internal standard and the acquisition time was 200 s. The trueness of both techniques was evaluated through the standard addition method, the recoveries obtained by SRTXRF and EDXRF were 76 and 99%, and the limits of detection, 13 and 240 µg l^?1, respectively. Copyright © 2011 John Wiley & Sons, Ltd.     

The hoard of Beçin—non-destructive analysis of the silver coins

We report the results of an analytical investigation on 416 silver-copper coins stemming from the Ottoman Empire (end of 16th and beginning of 17th centuries), using synchrotron micro X-ray fluorescence analysis (SRXRF). In the past, analyses had already been conducted with energy dispersive X-ray fluorescence analysis (EDXRF), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM/EDX) and proton induced X-ray emission spectroscopy (PIXE). With this combination of techniques it was possible to confirm the fineness of the coinage as well as to study the provenance of the alloy used for the coins.     

Determination of gold and silver in dross using EDXRF technique

Gold and silver in dross were determined by energy‐dispersive X‐ray fluorescence technique. Sample was prepared by pressed pellet method using microcrystalline cellulose powder as binder, and a method of standard additions was used for quantification. L_β X‐ray of gold (11.4 keV) and K_β X‐ray of silver (24.9 keV) were used for analysis. The measured concentrations of gold and silver were 132 ± 8 and 1181 ± 84 mg kg^?1, respectively. The results were validated by instrumental neutron activation analysis technique. The t‐test indicated that there was no significant difference between results obtained by the two techniques. Energy‐dispersive X‐ray fluorescence is a simple, precise and accurate technique for the determination of gold and silver in dross. Copyright © 2014 John Wiley & Sons, Ltd.     

Detection limits of high temperature superconducting materials on various substrates by energy dispersive X-ray fluorescence and proton induced X-ray emission methods

Application of energy dispersive X-ray fluorescence (EDXRF) and proton induced X-ray emission (PIXE) methods has been demonstrated for determining the elemental composition of thin film superconducting materials. The results of analysis carried out by EDXRF method have been compared with those obtained by PIXE method. Thin films of YBa₂Cu₃O₇ superconducting material were deposited on various substrates such as thin mylar sheet and thick substrates of SrTiO₃, MgO and Al₂O₃. In thin backing the minimum detection limits obtained for Cu, Y, Ba by the PIXE method are 20 ng, 70 ng and 800 ng respectively and the corresponding values by the EDXRF method are 3000 ng, 600 ng and 1000 ng. Detection limits for samples on thick backings deteriorated to a large extent by both methods.     

EDXRF determination of impurities in potassium dihydrogenphosphate single crystals and raw materials

A fast and simple preconcentration procedure for recovering various cation impurities from potassium dihydrogenphosphate (KDP) single crystals and raw materials, followed by energy‐dispersive X‐ray fluorescence analysis (EDXRF), is described. The technique is based on the adsorption of metal 8‐hydroxyquinoline complexes from aqueous solutions of KDP on activated carbon, separation of the concentrate on a Nuclepore filter and subsequent determination by EDXRF. To fix activated carbon powder on a filter surface, an amount of 1‐hexadecanol is added to the KDP solution during the preconcentration procedure. The optimum conditions for the best recovery of the impurities were established. It was shown that a preconcentration factor of 100 can be achieved and the detection limit for a number of elements was down to 0.01 µg g^?1. The relative standard deviations were 6–17% for element concentrations of 0.2 µg g^?1. The method was successfully applied to the determination of Fe, Co, Cu, Ni, Zn, Mn, Ti and Bi in KDP single crystals and raw materials. Copyright © 2005 John Wiley & Sons, Ltd.     

Energy dispersive X‐ray fluorescence analysis of archeological metal artifacts from the Final Bronze Age

Energy dispersive X‐ray fluorescence (EDXRF) is widely used in the study of archeological metal artifacts, heritage and art history, where the fragile nature of the objects requires the use of noninvasive techniques such as the EDXRF, which in addition, is fast and very affordable. An EDXRF analysis of copper‐based artifacts from Late Bronze Age metal hoards from Central Portugal is presented. The EDXRF measurements were carried out by using an X‐ray tube with a Mo anode and a commercial Si‐PIN detector. The data acquisition was performed by keeping small distances between the X‐ray window, the sample and the detector. Both patinated and polished areas were analyzed: the relative composition of the artifacts was inferred from the fluorescence spectra obtained. Copyright © 2012 John Wiley & Sons, Ltd.     

Room temperature ferromagnetism in nanocrystalline Ni-doped ZnO synthesized by co-precipitation

Ni-doped ZnO powder was synthesized by thermal co-decomposition of a mixture of bis(acetylacetonato) zinc(II)hydrate and bis(dimethylglyoximato)nickel(II) complexes. The samples were characterised by X-ray diffraction (XRD), Energy dispersion X-ray fluorescence (EDXRF), and FT-IR spectroscopy. The atomic ratio Ni/Zn of the samples was determined by the EDXRF method to be 1%, 4.3%, 7.4% and 22.5 wt%. The XRD studies show the formation of nanocrystalline (14-18 nm) of Ni-doped ZnO along with nanoparticles of NiO. By magnetic measurements, it was observed that powder contains 1%Ni, 4.3%Ni, 7.4%Ni exhibits superparamagnetic behaviour while the sample of 22.5%Ni prepared in closed atmospheric environment shows clear ferromagnetic (FM) loop at room temperature due to the formation of solid solution Zn_1−xNi_xO.     

Large scale synthesis of cadmium selenide nanowires using template synthesis technique and their characterization

We report the fabrication, and structural and optical characterization of CdSe nanowires. Large scale uniform nanowires with length 40 micron and diameter 100 nm were grown using the simple chemical reaction technique. Morphological study of CdSe nanowires was done using scanning electron microscopy (SEM). X-ray diffraction (XRD), and Raman studies show the crystalline structure of CdSe nanowires. Energy dispersive X-ray fluorescence (EDXRF) technique was used to study the composition of CdSe nanowires. UV–Vis absorption studies show a blue shift of 0.26 eV in the optical band gap of CdSe nanowires.     

A Practical Method for the Analysis of Overlapped Peaks in Energy Dispersive X-Ray Spectra

ABSTRACT

In this study a practical method for the spectral analysis of some overlapped characteristic X-ray peaks is presented. The overlapped characteristic K, and K, peaks and the artificially overlapped two K, peaks (peak doublet) of arsenic obtained by the radioisotope-excited, energy dispersive X-ray fluorescence (EDXRF) technique, are resolved. A total of 34 overlapped peak systems were investigated: the proposed method provided 18 reliable results, whereas the first and the second methods gave 15 and 1, respectively. The intensity ratios of K_β/K_α, obtained by the novel method are also in good agreement with the theoretical relativistic Hartree-Slater values.     

Preconcentration of mercury on polyaniline expands the horizon for energy dispersive X‐ray fluorescence determination

Hg(II) was sorbed on polyaniline from aqueous solutions, followed by determination using energy dispersive X‐ray fluorescence spectrometry. Distribution coefficient of Hg(II) on polyaniline was about 4 × 10³ in water, whereas distribution coefficient was 1.2 × 10⁴ at 0.1 M HCl and decreased drastically with increase in HCl concentration. Rapid kinetics of sorption was evinced by the 80% uptake within the initial 1 min and quantitative sorption within 5 min of equilibration. The sorption was found to follow Langmuir isotherm model, and the Langmuir capacity was calculated as 19.7 mg g^?1. The ability of polyaniline to form stable and homogeneous pellets facilitated the energy dispersive X‐ray fluorescence determination without recourse to elution. Detection limit of Hg was found to be 22 ng, considering 100 mg pellet of polyaniline. The apparent detection limit was 6 pg, as the preconcentration factor of Hg(II) on polyaniline was 4 × 10³. The developed method is at par with the established method for mercury determination, namely, cold vapor atomic absorption spectrometry. Accuracy of the method was established by the analysis of the International Atomic Energy Agency reference materials, namely, hair and lichen, for Hg(II). Copyright © 2016 John Wiley & Sons, Ltd.     

Assessment of chemical elements in cosmetics' eyeshadows by X‐ray fluorescence and International Nomenclature of Cosmetic Ingredients characterization

Energy dispersive X‐ray fluorescence (EDXRF) technique, as a qualitative and quantitative analysis, was used for inorganic chemical elements determination (K, S, Cl, Al, Si, Ca, Ti, Mn, Fe, Pb, Zn, Rb, and Bi) in eyeshadows for safe human use. International Nomenclature of Cosmetic Ingredients standardized nomenclature was used for labels investigation to obtain data on legal regularity. Data of 23 samples were clustered by similarity, measuring relative concentrations of detected chemical elements. Calculating the correlation among such values, a similarity matrix was used to generate a dendrogram. Pb was found in samples silver color S12E and copper color S22I above permissible limits (20 μg/g). Same composition was reported for the pink (S01A), black (S02A), and brown (S03A) samples, but the same chemical elements were not detected by EDXRF in them. The best correlation was found between samples S08D and S23 J (0.961). The least correlation was 0.0012 between S01A and S12E. The clustering analysis showed 7 groups of similar samples according to EDXRF data. Relations among 6 eyeshadows' colors and chemical compositions were discovered by using decision trees, where the most determinant elements were Mn, S, Cl, Ca, and Fe, in this order. Commercial regularization and International Nomenclature of Cosmetic Ingredients standardization of eyeshadows in Brazil are not fully complied by the manufacturers of the investigated brands.     

能量色散X荧光分析中元素间效应的蒙特卡罗模拟

针对能量色散X荧光分析(EDXRF)技术中元素间效应实验研究的难点问题,采用蒙特卡罗方法对基于Si（PIN）探测器的EDXRF系统建立模拟模型,并对模拟微束软X射线注量谱建立了高斯展宽算法。对Fe-Ni样品进行模拟计算,表明经该算法展宽后的注量谱与实测K系特征X射线谱吻合度较高,并得到了各元素特征X射线归一计数与元素含量关系曲线,结果表明该方法可自行校正EDXRF中元素间效应,获得准确的元素K系特征X射线谱理论强度。     

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.     

Microchemical surface analysis of two Numidian coins

This work is a contribution to the microchemical surface analysis of two Numidian coins. Numidia was an ancient kingdom of northern Algeria during 2nd and 1st century BC. Investigations were performed with scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS), energy dispersive X-ray fluorescence spectrometry (EDXRF) and X-ray diffraction (XRD). The identification of the coins was done thanks to the name initials and effigy of King Massinissa. SEM observations of coins showed heterogeneous surfaces. SEM and EDXRF analyses showed an alloy structure with copper (65%), antimony (19%) and lead (16%). The XRD identified a metal structure and corrosion products which were on the coin surfaces: Litharge (PbO), Hydrocerussite (Pb₃(CO₃)₂(OH)₂), Bindheimite (Pb₂Sb₂O₇) and Bystromite (MgSb₂O₆).     

An alternative method for the determination of element concentrations in schizophrenic, lung cancer and leukaemia patient bloods

Concentration of the elements present in schizophrenic, lung cancer and leukaemia patients’ bloods were determined using energy-dispersive X-ray fluorescence (EDXRF) method. EDXRF spectrometer with an annular and sources was applied for the analysis of blood samples. A sample preparation procedure suitable for the EDXRF, the experimental approach, analytical method used in this study and the results were presented. EDXRF technique has been successfully used for the determination of elements present in blood.     

X‐ray fluorescence spectrometry in Dar es Salaam

Energy‐dispersive x‐ray fluorescence (EDXRF) analysis has been established at the University of Dar es Salaam, Faculty of Science, Department of Physics. Calibration was conducted using thin films from Micromatter (USA) for secondary target XRF. We report on the performance of the spectrometer including the detection limits attained, which range from 0.01 to 10 ng cm^?2 using collimators of 6 and 8 mm diameter under excitation conditions of 50 kV, 35 mA. The accuracy of the measurements was checked using IAEA SOIL‐7 and NIST 3087a Certified Reference Materials. The experimental values differed by <5% from the certified values. The total reflection x‐ray fluorescence (TXRF) facility added as a module to the existing XRF system provides detection limits between 0.1 and 100 pg for most of the elements measured. Copyright © 2005 John Wiley & Sons, Ltd.     

波长与能量色散复合式X射线荧光光谱仪特性研究及矿区土壤分析

波长与能量色散(WD-ED)复合式X射线荧光(XRF)光谱仪是一型国际上新近研发的XRF光谱仪。该研究比较了此型光谱仪的特性,建立了联用分析方法,并用不确定度对所建方法进行了评估,证明WD-EDXRF复合型光谱仪及其所建分析方法可用于土壤样品中主、次、痕量元素定量测定,并兼具了WD和ED各自的优点。研究表明：(1)对土壤质量和生态环境评价中具有重要意义的Mg,Al,P和K等元素,因WDXRF对轻元素具有更高灵敏度,故采用该型光谱仪和所建方法,可弥补单一采用ED方法的不足,从而为土壤质量和生态环境评价提供了更为灵敏和准确可靠的分析技术手段;(2)在本方法实验条件下,采用WDXRF测定,主元素Na₂O,MgO,Al₂O₃,P₂O₅,K₂O的检出限优于EDXRF,而SiO₂, SO₃, CaO, MnO, Fe₂O₃则是由EDXRF测定的检出限更优。对于谱线重叠较严重的微量元素,多数情况下WDXRF的检出限更低;(3)对主元素而言,总体上K及其原子序数之前的轻元素WDXRF准确度更好,Ca及其之后的元素EDXRF准确度更好。然而,由WDXRF和EDXRF获得的准确度也与样品相关,在某些情况下,EDXRF测定K的准确度会更好。微量元素和重叠干扰比较大的元素,采用分辨率好的WDXRF可获得更好的准确度;对于受其他元素谱线重叠影响较小的元素,EDXRF给出的结果准确度更好;(4)选用添加石蜡粘结剂的粉末压片法,利用该方法制成的地质样品粉末压片结实、无脱落,未观察到掉渣、掉粉现象,且分析准确度和精密度良好;(5)利用所建立的WD-EDXRF方法测定了采自集中开采矿区和附近河流及河漫滩沉积物,揭示矿区表层土含有较高浓度的Cu,Pb和Zn,可为找矿提供指示信息;(6)进行了矿区周边农田土壤分析,获得了元素分布趋势图,揭示矿集区附近农田土壤Pb和As等浓度较高,需要采取必要的生态与环境保护措施,以减小和避免对于人类健康的潜在影响。