EDXRF Spectrometer Research Articles

Effect of Organic Waste on Crystal Structure and Mechanical Properties of Concrete

The influence of organic waste as an additive to concrete formulation has been studied by replacing up to 10% of cement ratio with locally sourced organic additive. The reference cement used was Portland cement; three different organic wastes were used in the mixture: periwinkle shell, extracted silica from corn hob ash and coconut shell ash. Uniform distribution of the additive was ensured by thorough mixing prior to water addition. Casting and curing of the concrete were done in line with established standard. The compressive strength test was carried out using the Instron universal testing machine and the oxides of elemental composition of the cement and the additives were determined using EDXRF Spectrometer (EDX 3600B) while the crystallography studies were carried out using EMMA) X-ray diffractometer . The result obtained indicated that there was a significant difference between the value of density, packing efficiency and compressive strength of each reinforced concrete with that of the reference cement which was attributable to the presence of additives. The cement formulation with silica as admixture was found to have the highest compressive strength of 217.94 MPa, while the reference cement had the lowest compressive strength of 81.45 MPa. This study has established that locally sourced organic additives (emerging additives), influence the mechanical properties of concretes.

Evaluation of uncertainty in the energy dispersive X-ray fluorescence determination of platinum in alumina

Uncertainty, the most important characteristic of an analytical result, has been evaluated using a bottom-up approach during EDXRF determination of Pt in alumina. The calibration function of the EDXRF spectrometer was derived through bivariate least squares fitting, in combination with weighted regression of the residuals.

The Potential of a Portable EDXRF Spectrometer for Gemmology

The Potential of a Portable EDXRF Spectrometer for Gemmology

Environmental nuclear-geophysical ore monitoring in mines of Corporation Kazakhmys PLC

An environmental monitoring of ore composition in complex deposits of Kazakhstan (the Zhezkazgan, Kusmuryn, Artemjevsk, Kounrad, Taskura and Zhaman-Aibat deposits) is carried out using EDXRF spectrometers RPP-12, RLP-21 and RLP-21T. The monitoring of ore concentrates in Satpaev, Balkhashsk and Zhezkazgan processing plants and in Zhezkazgan copper smelter continues at present time. The monitoring suggests data on new promising elements and environmental pollutants in ores and new trends in distribution of bound elements in ores.

Scientific analyses beyond the excavation: studies for a non invasive preliminary approach

Domo is an archaeological site located in the Foreste Casentinesi National Park, near the town of Bibbiena, in the province of Arezzo (Tuscany). Since the ’80, investigations at Domo have revealed a Roman domus with a Roman baths complex. Unfortunately, the rich stratigraphy was almost completely lost during the first excavations. Since 2008 the archaeological site was reopened by Archeodomani s.a.s., a company that deals with promotion of cultural heritage, and it is still under summer excavation campaigns. In the future perspective to try and solve doubts about the site phase sequence of the Roman baths complex, not easy to understand now for several use modifications of the different areas, we developed an analytical method that could allow a large scale investigation limiting the sampling. In this paper, we present the preliminary results obtained for mortar, both from the walls and from the binding of cocciopesto, with XRD (X Ray Diffraction) and ED-XRF (Energy Dispersive X-Ray Fluorescence) analysis on ground samples. XRD analysis was performed at ICVBC-CNR and the diffraction data (Cu–Ka, 1.5418 A) were collected on a J-J Panalytical X’Pert PRO spectrometer. Grounded samples were placed in aluminium sample holder or dusted on frosted glass sample holder, depending on sample amount. XRF measurements were performed at Physics Department of Milan University using a portable EDXRF spectrometer (Assing Lithos 3000) exploiting polychromatic radiation from a Mo anode X-ray tube. Both analyses were performed after preliminary observation of the samples by stereo-microscope and the results obtained through XRF and XRD were compared to get more complete information about samples. Data were also submitted to multivariate analysis (Hierarchical Clustering) to get material classification. The comparison between the classification obtained and archaeological interpretation is still in progress; the collection of analytical data will go on in future excavation campaigns. The complete overview will be part of a project to promote the archaeological site through an online portal.

Investigation of the mass loss of water soluble ionic compounds caused by EDXRF analysis of PM10 loaded filters

The mass loss of particulate matter (PM) due to EDXRF analysis was gravimetrically evaluated on co-located PM10 loaded filters analyzed both using EDXRF under vacuum and using Ion Chromatography. Then, this comparison was repeated with air and helium (He) instead of evacuating the measurements chamber of the EDXRF spectrometer. It was shown that EDXRF application using vacuum medium led to mass loss of water soluble ionic compounds and other volatile constituents of PM10. The use of a He and air medium considerably reduced the PM mass losses. It is demonstrated that the mass loss of PM and ionic compounds mainly resulted from vacuum medium and from a lower extent to the level of X-ray energy. The influence of EDXRF application using vacuum medium on the mass losses of ionic compounds were further investigated. Different amounts of NO3−, NH4+, Cl−, Na+, Mg++ and Ca++ were lost whereas SO4−− and K+ remained unchanged. The relationship between vacuum and application time was also studied for quartz and Teflon filters. The longer the application time, the higher the PM mass loss was observed. The mass loss of PM on quartz filter was shown by experiments to be 2 times higher than on Teflon filter.

An estimation of EDXRF spectrometer properties, based on a two‐layer composite Si‐Ge detector

A mathematical model for the two‐layer composite Si‐Ge energy dispersive X‐ray detector is proposed, based on analyses of radiation and electron transport in the detector, and a mathematical model of an energy dispersive X‐ray fluorescent spectrometer with the detector is considered. The Monte Carlo method is applied to calculate probabilities of photon detection in different parts of the detector's response function. The composite detector with the time anti‐coincidence scheme is proposed; its first layer is Si detector, and the second layer is Ge detector. It is shown that this composite detector has some advantages, such as reduced Ge photo escape peaks intensities and efficiency of detection of high energy photons similar to efficiency of Ge detector. Applying the X‐ray detector for the energy dispersive X‐ray fluorescent spectrometer provides for a lower background level. Copyright © 2012 John Wiley & Sons, Ltd.

Direct rapid analysis of trace bioavailable soil macronutrients by chemometrics-assisted energy dispersive X-ray fluorescence and scattering spectrometry

Precision agriculture depends on the knowledge and management of soil quality (SQ), which calls for affordable, simple and rapid but accurate analysis of bioavailable soil nutrients. Conventional SQ analysis methods are tedious and expensive. We demonstrate the utility of a new chemometrics-assisted energy dispersive X-ray fluorescence and scattering (EDXRFS) spectroscopy method we have developed for direct rapid analysis of trace ‘bioavailable’ macronutrients (i.e. C, N, Na, Mg, P) in soils. The method exploits, in addition to X-ray fluorescence, the scatter peaks detected from soil pellets to develop a model for SQ analysis. Spectra were acquired from soil samples held in a Teflon holder analyzed using 109Cd isotope source EDXRF spectrometer for 200s. Chemometric techniques namely principal component analysis (PCA), partial least squares (PLS) and artificial neural networks (ANNs) were utilized for pattern recognition based on fluorescence and Compton scatter peaks regions, and to develop multivariate quantitative calibration models based on Compton scatter peak respectively. SQ analyses were realized with high CMD (R2>0.9) and low SEP (0.01% for N and Na, 0.05% for C, 0.08% for Mg and 1.98μgg−1 for P). Comparison of predicted macronutrients with reference standards using a one-way ANOVA test showed no statistical difference at 95% confidence level. To the best of the authors’ knowledge, this is the first time that an XRF method has demonstrated utility in trace analysis of macronutrients in soil or related matrices.

Li(i=1–3) sub-shell x-ray relative intensities for some compounds of 66Dy at 22.6 and 59.54 keV incident photon energies

The intensity ratios, ILk/ILα (k=l,β1,4,β3,6,β2,7,9,10,15,γ1,5,γ2,3,γ4,β,γ), have been measured for some compounds of 66Dy, namely, Dy2O3, Dy2(CO3)3, Dy2(SO4)3, DyI2 and Dy metal by creating the Li(i=1–3) sub-shell vacancies in widely different proportions at two incident photon energies of 22.6keV and 59.54keV, in order to check the predicted dependence of these ratios on the incident photon energy and also investigate the influence of chemical effects on these ratios for an f-block element. The measurements were performed using the EDXRF spectrometer involving disk type radioactive sources of Cd109 and Am241 and a Peltier cooled Si PIN x-ray detector arranged in the 90° reflection geometry. The measured intensity ratios have been compared with the theoretical ILk/ILα values and those calculated using the two sets of fluorescence and Coster–Kronig yields available in literature in order to check the reliability of the theoretical/calculated values. Further, the measured ratio, ILγ4/ILα, was found to depend on the oxidation state of 66Dy as well as nature of ligand attached to it in a given compound.

Fast and simple method for determination of fatty acid methyl esters (FAME) in biodiesel blends using X-ray spectrometry

The determination of fatty acid methyl esters (FAME) in diesel fuel blends is an important aspect of production and blending process as well as quality control of distribution operations. In this study, energy-dispersive X-ray fluorescence spectrometer (EDXRF) is used for the first time for determination of FAME in biodiesel blends. The principle of the method is based on intensity difference of X-ray radiation scattered from hydrocarbons and from FAME. The experiment shows that coherent and incoherent radiation, commonly applied for evaluation of the average atomic number of the sample with light matrix, cannot be applied for FAME determination. However, the application of scattered continuous radiation gives excellent correlation between FAME concentration and intensity of scattered radiation. The best results are obtained if continuum is collected in the range of energy between 10.5 and 15.0keV for rhodium X-ray tube, operated at 35kV. Linear relationship between the FAME concentration and the inverse of scattered continuous radiation is obtained with the correlation coefficients of 0.999. Standard deviation of measurement is ca. 0.46% (v/v) of FAME and detection limit is 1.2% (v/v) for 600s counting time and 50% dead-time loss using Si-PIN detector. The investigation shows that crucial issue in determination of FAME in biodiesel blends using EDXRF spectrometer is the precision of measurements resulting from the counting statistics. Therefore, much better results (0.20% (v/v) standard deviation and 0.52% (v/v) detection limit) can be expected if higher intensity of primary radiation is applied and X-ray spectrum is collected by silicon drift detector of high input count rate. For concentration of FAME from 10 to 100% (v/v), the differences between reference method (Fourier transform infrared spectrometry) and the proposed method usually do not exceed 1% (v/v) of FAME. The proposed method is fast, simple and enables FAME determination in wide range of concentration up to 100% of FAME without any sample treatment.

Chemical effects on the L i( i=1–3) sub-shell X-ray relative intensities for some compounds of Hg

The intensity ratios, I L k / I L α (exp) ( k= l, η, β 4,6, β 1,2,3,15, β 5,7, γ 1,5, γ 2,3,6,8, γ 4, β, γ), have been measured for some compounds of 80Hg, namely, HgI 2, Hg(C 2H 3O 2) 2 and a pure 80Hg target (liquid form) at 22.6 keV incident photon energy in order to investigate the influence of chemical effects on these ratios for a heavy transition element. The measurements have been performed using the EDXRF spectrometer involving a disk type radioactive source of Cd 109 and a Peltier cooled Si-PIN X-ray detector arranged in the 90° reflection geometry. The measured intensity ratios have been compared with the theoretical I L k / I L α (Thr.) values ( Kumar et al., 2010) and those calculated using the fluorescence and Coster–Kronig yields tabulated by Campbell (2003, 2009) and Krause (1979) in order to check the reliability of these available values. The measured ratios, I L β5,7 / I L α (Exp.), were found to be influenced by the chemical effects.

Speciation of heavy metals (Cu, Pb, Ni) pollutants and the vulnerability of groundwater resource in Okrika of Rivers State, Nigeria

The chemical mobility of heavy metal pollutants (Cu, Pb, and Ni) is fundamental to the understanding of their environmental accessibility, toxicity and geochemical behaviour to be able to account for the safety and vulnerability of the groundwater resource in the study area. In this work, EDXRF spectrometer was used to determine the total concentration of the metals in the samples and the concentrations left in the residual fractions after extraction. FAAS was used for the chemical analysis of the test sample extracted. The results show that the concentrations of the mobilized fractions are well within the permissive limit, and more of the concentrations of about 60% to 80% of the total concentrations of the pollutants are in the residual phase that keeps the pollutants in their inert state as such posed no threat to the environment and man, and particularly rendering the groundwater resource less vulnerable to the presence of these pollutants. There remobilization is very possible under favourable conditions as therefore, constant monitoring of human activities should be put in place with regular evaluation of pollution status of the environment for the good of all.

Use of TXRF and Convectional Energy Dispersive X‐ray Fluorescence Analysis (EDXRF) to determine trace metal concentrations in waters of Nakivubo Channel and Lake Victoria

To understand better the pollution levels in the waters of the Nakivubo Channel and Lake Victoria, the concentrations of manganese (Mn), iron (Fe), cobalt (Co), copper (Cu), zinc (Zn) and lead (Pb) were determined using convectional Energy Dispersive X-ray Fluorescence Analysis (EDXRF) and Total X-ray Fluorescence (TXRF) analysis. Particulate deposits were analysed for trace metals with a convectional EDXRF spectrometer. Extracted dissolved metals contents were analysed with Total Reflection X-Ray Fluorescence. The analyses indicated higher copper concentrations in the filtrate samples collected at the rivermouths and inshore stations than on the particulate matter. Samples from battery manufacturing industry-1 indicated copper concentrations in the filtrate exceeding the National Environmental management Authority (NEMA) drinking water standard of 1.0 mg L−1. Free zinc concentrations were measured for almost all the sampling sites, but at concentrations below the 3 mg L−1 NEMA standard. High concentrations of iron in the labile form measured at the lake shores were above NEMA drinking water standards of 0.3–3.5 mg L−1 in 2006, except for the April 2006 Murchison Bay rivermouth, and for low manganese concentrations in the lake waters. The iron and manganese concentrations on the particulate matter at the upstream end of the Channel, but were lower in the lake waters. Effluents from soap manufacturing industries exhibited elevated total iron concentrations, ranging from 19.038 ± 0.190 to 63.129 ± 6.248 mg L−1 throughout the 2-year study period. The manganese concentrations were the highest for the battery manufacturing industry-2 site in April 2006. The total iron and manganese concentrations were generally higher upstream along the Nakivubo Channel than in the lake waters. Cobalt and lead concentrations were below detection limits for most of the sampling sites. Generally, most metal concentrations along the Nakivubo Channel exceeded acceptable limits, illustrating the need for mitigation measures.

Comparison of three portable EDXRF spectrometers for pigment characterization

AbstractIn the field of cultural heritage analyses, energy dispersive X‐ray fluorescence is a well known nondestructive technique used—among other applications—to characterize pigments and inks in artifacts such as paintings, polychromous sculptures and illuminated manuscripts. In this paper, we report on the performance of three portable X‐ray fluorescence analyzers currently used for laboratory or in situ analyses. The three spectrometers have been tested in laboratory on paint layers prepared to simulate real ones, with the specific goal to determine advantages and disadvantages for each instrument in the detection of specific elements characterizing the pigment. Additionally, overall general advantages and limitations of each system in practical use are highlighted. Copyright © 2010 John Wiley & Sons, Ltd.

Oxford Instruments launches a powerful, new, easy-to-use EDXRF spectrometer – designed for operation by anyone!

Oxford Instruments launches a powerful, new, easy-to-use EDXRF spectrometer – designed for operation by anyone!

Applicability of MiniPal 4 compact EDXRF spectrometer for soil and sediment analysis

AbstractOptimum measurement parameters for analysis of soil and sediment samples with the compact MiniPal 4 (MP4)EDXRF spectrometer (PANalytical, Almelo, The Netherlands) were presented. The following elements were considered: K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As and Pb. Since the elements from low Z to medium Z region were covered, three measurement conditions (sequences) were defined. The following parameters were selected for measurement of the elements K, Ti, and V: voltage = 12 kV; current = 750 µA; filter material: Al_thin. Cr, Mn and Fe were measured at 20 kV; 300 µA with Al filter while for measurements of Ni, Cu, Zn, As, Pb, Rb, and Sr an Ag filter was selected and tube voltage and current were 30 kV and 300 µA. Each sequence was measured for 200 s and measurements were done in the air. MP4 spectrometer was characterized with acceptable precision, long‐term stability and satisfactory minimum detection limit for the analyses of soil and sediment materials. For the elements K, Mn, Fe, and Ti the precision of the analysis was better than 0.5% and for all the other elements better than 5%. Detection limits for sediment samples were 20 ppm for K, 6.1 ppm for Ti, 5.2 for Mn, 4 ppm for Fe, 4.2 ppm for As and less than 2 ppm for all the other elements. These values were significantly lower compared to typical concentrations of the same elements found in unpolluted soil and sediments. Copyright © 2008 John Wiley & Sons, Ltd.

L i ( i = 1–3) subshell X-ray production cross sections and fluorescence yields for some elements with 56 ⩽ Z ⩽ 68 at 22.6 keV

The L k ( k = l, α, β 1,4, β 3,6, β 2,15,9,10,7, γ 1,5 and γ 2,3,4) X-ray production (XRP) cross sections have been measured for six elements with 56 ⩽ Z ⩽ 68 at 22.6 keV incident photon energy using the EDXRF spectrometer. The incident photon intensity, detector efficiency and geometrical factors have been determined from the K X-ray yields emitted from elemental targets with 22 ⩽ Z ⩽ 42 in the same geometrical setup and from knowledge of the K XRP cross sections. The L 1 and L 2 subshell fluorescence yields have been deduced from the present measured L k XRP cross sections using the relativistic Hartree-Fock-Slater (HFS) model based photoionization cross sections. The present deduced ω 1 (exp) values have been found to be, on an average, higher by 15% and 20% than those based on the Dirac–Hartree–Slater (DHS) model and the semi-empirical values compiled by Krause, respectively, for elements with 60 ⩽ Z ⩽ 68.

Micro-EDXRF surface analyses of a bronze spear head: Lead content in metal and corrosion layers

A bronze spear head from Central Portugal dated to Late Bronze Age has been analyzed by non-destructive micro-EDXRF in the metal surface and corrosion layers. The artifact had previously been analyzed using a conventional EDXRF spectrometer having a larger incident beam. The quantification of the micro-EDXRF analyses showed that lead content in corrosion layers can reach values up to four times higher than the content determined in the metal surface. Results obtained with the higher energy incident beam from the EDXRF equipment, although referring mainly to the corrosion layers, seem to suffer some influence from the surface composition of the metallic alloy.

Spatial XRF distribution characteristics associated with polarized EDXRF spectrometry

AbstractAn experiment was designed and carried out to measure the XRF yield distribution over the area irradiated by the target's x‐rays in a polarized EDXRF spectrometer. A small solder disc, which was made of mainly lead and tin and with a diameter of about 3 mm, was scanned manually with equal displacements over the area. XRF spectra excited by radiation from three typical targets, namely, highly oriented pyrolytic graphite (HOPG), Mo and Al2O3, were collected. Intensities of Sn Kα and Lα and Pb Lα and Mα lines were obtained and used to describe the XRF yield distributions from different targets. The results showed that the total areas contributing to the XRF signal were over 2 cm2 for the above three targets. Also, Pb Mα and Sn Kα maps irradiated by HOPG and Al2O3, respectively, showed very high intensities in the central parts, while they were very low in the periphery. The sum of intensities from four spots in central area (corresponding to about 7 × 7 mm2) represents about 50% of overall integrated intensities of the 33 measured spots. Also, the sharpest areas of Pb Mα and Sn Kα were slightly shifted. Pb Lα maps obtained using the Mo target showed much larger distribution areas, with center being the most intense and becoming weaker gradually toward the outer parts. The relatively small irradiation areas of the polarized targets may require better sample homogeneity, and care should be taken when small pieces of samples are to be analyzed. Copyright © 2007 John Wiley & Sons, Ltd.

Portable EDXRF analysis of a mud brick necropolis enclosure: evidence of work organization, El Hibeh, Middle Egypt

The geochemical and sedimentological compositions of mud brick from a feature called the Square Enclosure in the eastern desert necropolis of the ancient town site of El Hibeh, Egypt, were investigated along with surface sediments from the local Nile floodplain for the purpose of establishing possible sources of the mud brick. Geochemical examination was undertaken with a portable EDXRF spectrometer; a field portable sedimentological laboratory was used to collect grain size, mineralogy, and strength analysis data. Results of the analyses produced evidence of work organization relating to the construction of the Square Enclosure. This discovery is the first archaeological evidence of work organization from the mud brick of ancient Egyptian structures and provides a valuable contribution to our knowledge of ancient Egyptian work organizational practices.