Energy Dispersive X-ray Fluorescence Spectrometry Research Articles

Producing hybrid fuels by hydrotreating Jatropha curcas L. and gasoil mixtures in a batch reactor

The co-processing of Jatropha curcas L oil (JC) and gasoil in mixtures of 20:80 and 50:50 volume percentages, respectively, was carried out in a batch reactor by using a commercial NiMo/Al2O3 (5wt%) catalyst at 750 rpm, 70 bar of initial pressure and 80/100 mesh particle size. The effect of temperature (370-390 °C) at fixed reaction time of 4 h in the oxygen and sulfur removals were followed with Fourier Transform Infrared Spectroscopy, Proton Nuclear Magnetic Resonance and Energy Dispersive X-ray Fluorescence Spectroscopy. Also we use simulated distillation to determine the boiling point distributions. It was found that 98 and 99 % conversions of vegetable oils were obtained for 20 and 50 vol% JC feedstocks and similar ∼ 83 and 87 % hydrodesulfuration (HDS) conversions for both fossil-vegetable mixtures at 380 and 390 °C. However at 370 °C the attained HDS conversion was more than 10% lower in mixture with 50 vol% JC. Regarding boiling point distributions, yields averaging 58 vol% and 70 vol% of cut with boiling range 157-343 °C, were obtained with 20 vol% and 50 vol% JC feed mixtures, respectively.

Evaluation of ecological risk, source, and spatial distribution of some heavy metals in marine sediments in the Middle and Eastern Black Sea region, Turkey.

In the present study, the concentration levels of heavy metals such as Mn, Fe, Ni, Cu, Zn, Cr, and Pb in sediment samples collected from 16 sampling locations in the Middle and Eastern Black Sea regions, Turkey, were measured using energy dispersive X-ray fluorescence spectroscopy (EDXRF). Various pollution parameters and methods, such as the enrichment factor (EF), geo-accumulation index (Igeo), contamination factor (CF), pollution load index (PLI), ecological risk index (RI), and geo-spatial distribution patterns, were used to assess the pollution status, ecological risks, and sources of metals in sediment in detail. The mean concentrations of Mn, Fe, Ni, Cu, Zn, Cr, and Pb were found to be 565.38, 46,000, 34.38, 104.06, 109.88, 87.31, and 32.31 mg/kg, respectively. Results showed that the mean concentrations of Cu, Zn, and Pb exceeded the crustal shale value, with the exception of Mn, Fe, Ni, and Cr. According to the calculated pollution parameters, although minimal or moderate pollution was detected in the area investigated, it was determined that there was a very low ecological risk. Multivariate statistical analysis results showed that Cu, Zn, and Pb levels in the investigated region were slightly influenced by anthropogenic inputs such as mining and agricultural practices. In addition, the geo-spatial distributions of Cu, Zn, Fe, and Pb were found to be higher in this region due to the mining activities carried out in the Eastern Black Sea region.

A Highly Efficient Environmental-Friendly Adsorbent Based on Schiff Base for Removal of Cu(II) from Aqueous Solutions: A Combined Experimental and Theoretical Study.

Removal of heavy metals from drinking water sources and rivers is of strategic health importance and is essential for sustainable ecosystem development, in particular in polluted areas around the globe. In this work, new hybrid inorganic-organic material adsorbents made of ortho- (Si-o-OR) or para-Schiff base silica (Si-p-OR) were synthesized and characterized in depth. These hybrid adsorbents show a high selectivity to Cu(II), even in the presence of competing heavy metals (Zn(II), Cd(II), and Pb(II)), and also demonstrate great reusability after five adsorption-desorption cycles. Maximum sorption capacity for Cu(II) was found for Si-o-OR (79.36 mg g−1) and Si-p-OR (36.20 mg g−1) in no less than 25 min. Energy dispersive X-ray fluorescence and Fourier transform-infrared spectroscopy studies demonstrate that this uptake occurs due to a chelating effect, which allows these adsorbents to trap Cu(II) ions on their surfaces; this result is supported by a theoretical study for Si-o-OR. The new adsorbents were tested against real water samples extracted from two rivers from the Oriental region of Morocco.

Energy-dispersive spectroscopy for the quantitative determination of the major chemical elements in milk

The present preliminary study aims at the rapid quantitative determination of the major chemical elements in the ashes of raw milk samples, using energy dispersive X-ray fluorescence spectrometry. The precision of the method was satisfactory (variation coefficient ≤ 5%). The mean values (in mmol·kg-1) obtained from the analysis of 32 raw milk samples showed good agreement with data from the Brazilian and international literature: K (26.1 ± 4.6), Ca (33.8 ± 3.7), P (28.4 ± 2.7), Na (21 ± 3.3) and Mg (4.7 ± 0.5). Residual Cl concentration (19.0 ± 3.3 mmol·kg-1) was lower than expected due to incineration losses. The results suggest a good application potential of the method for other dairy products.

Human Health Risk Assessment and Histopathological Alterations in Puntius sophore of Damsal Nala, Sukinda Chromite Valley, Odisha, India

The aim of the present study was to assess the concentration of potentially toxic metals (PTMs) like As, Cd, Cr, Cu, Fe and Pb in the Damsal Nala of Sukinda Chromite Valley, Jajpur of Odisha (India) and its subsequent histopathological lesions in the fish Puntius sophore. Energy Dispersive X-Ray Fluorescence (EDXRF) and Flame Atomic Absorption Spectroscopy (FAAS) methods were used to evaluate the concentrations of PTMs in the muscles of fish, Puntius sophore collected from different zones namely upstream discharge zone (UDZ) and upstream zone (UZ) of the Damsal Nala and control water bodies (CW). In the UDZ of Nala, the concentration of metals viz., Cd, Pb and Fe were 2 to 7 times, and Cr was 77 times higher than the maximum permissible limits recommended by WHO and FAO in the fish muscles. The values of Target Hazard Quotients (THQ) of all these 6 metals were <1 in CW and UZ, but in UDZ the THQ values of Cr and Fe were >1. Hazard Index (HI) for UDZ was 3.47, indicated the alarming concentration of metal which can pose serious risk to human health. Histopathological observations in liver and kidney of Puntius sophore collected from UDZ demonstrated the serious lesions, but mild damage in fish collected from UZ. These histological alterations and the health risk indices disclosed the effects of effluents of chromite mining and the impact on the ecological balance which may result into health hazards to the local human population who are maintaining their livelihood by consuming these fish as protein source.

Investigation of inks, pigments and paper in four Moroccan illuminated manuscripts dated to the eighteenth century

The heritage left by the Arab world in the history of science is directly related to the innovations in both the manufacturing of paper and the production of ink. Four Moroccan manuscripts dating to the eighteenth century, conserved at the royal library of Rabat, have been analyzed by X-ray diffraction (XRD), energy-dispersive X-ray fluorescence spectrometry (EDXRF), scanning electron microscopy coupled to energy dispersive X-ray spectroscopy (SEM–EDS), Raman and attenuated total reflection Fourier transformed infrared spectroscopy (FTIR-ATR). The combination of the Raman, EDS, and EDXRF spectroscopies results allows us to Characterized the inorganic inks, pigments and fillers used in paper making process. Iron-based ink was used for writing the text for all manuscripts. The main pigments used in the titles and in the illuminated part are found to be vermillion and red ochre in red samples, azurite with barium white and ultramarine in blue color, lead chromate in yellow color, copper and arsenic based ink in green color, carbon black for black color and gold. The main fillers identified in paper are calcite and kaolin. FTIR-ATR and Raman analysis revealed the presence of the characteristic bands of cellulose, the main component of paper. XRD confirms the presence of the fillers detected by FTIR-ATR. Finally, SEM allows to have a better knowledge of the typical morphology of the paper highlighting some effects of the degradation process.

Simple and rapid quantification of chromium, arsenic, and selenium in bituminous coal samples using a desktop energy dispersive X-ray fluorescence analyzer

In this study, the simple and rapid quantification of Cr, As, and Se in bituminous coal was achieved by energy dispersive X-ray fluorescence (EDXRF) spectrometry using pressed and powdered samples. The accuracy of the EDXRF method was improved by spectral processing optimization so the net intensity of the analytical X-ray line reflected the actual value. The EDXRF method provides results that are comparable to those obtained using traditional chemical analysis methods with two types of samples and it reduces the analysis time by 66% for pellet samples and 90% for powder samples.

Characterisation of Electroplated Gold Coatings for Dental Applications: Estimation of Thickness Using Non-Destructive Electron-Probe Microanalysis Related to Plating Time

Objectives: This study aimed to measure non-destructively gold (Au) electrodeposited on a high-gold alloy by modulating coating time and comparing this to sputtering Au to known thicknesses. Methods: Au was electrodeposited (plated) on 11 high-gold alloy plates (A–K) at 2.8V between 20 and 220 min. Seven Au strips were sputter coated on the same alloy to known thicknesses (range 50–500 nm). Energy dispersive X-ray spectroscopy (EDS) was used to measure minimal electron energy (E0) required to penetrate Au coatings and generate x-ray signals of 1% atomic palladium (Pd) from the underlying alloy for test samples and Au strips. % Pd X-ray concentration at maximum 30 kV was also obtained. The obtained signal–thickness relationship of known Au strip thicknesses was used to calculate Au thickness on the A–K samples based on two analytical relations. Energy dispersive X-ray fluorescence spectroscopy (XRF) was used as a complementary method to ensure coating thickness estimations were accurate. Results: EDS values for all reference and unknown thicknesses were obtained and verified with XRF. Correlating these signals with the Data Analysis Software and matching with known plating times allowed estimation of Au thickness of the unknown samples (range 27–425 nm). Estimated thicknesses were shown to have a linear relationship with plating time except for samples C–D, where there was an inverted relationship. Significance: A non-destructive method for measuring electrodeposited thickness of Au on high-gold alloys related to plating time was developed and verified. There is a linear relationship to Au thickness and plating time between 20 and 220 min.

Revealing Artists’ Collaboration in a 14th Century Manuscript by Non-Invasive Analyses

In the last decades, the working methods of late medieval illuminators have been widely discussed by art historians and codicologists. Non-invasive analyses are able to characterise the painting methods of illuminators as well as investigate artistic collaborations among them. The aim of this study was to characterise the painting palettes and techniques of different artists who illuminated two leaves from an early fourteenth century manuscript. The analyses were carried out with non-invasive and portable techniques such as Energy Dispersive X-ray Fluorescence (ED-XRF) spectrometry, Fiber Optics Reflectance Spectroscopy (FORS) and Raman spectroscopy. The paper highlights the differences among three rich and varied palettes and examines the pigments ultramarine, azurite, verdigris, earths, orpiment, red lead, vermillion, lead white, yellow lake, indigo, brazilwood and lac, used independently or in mixtures. We have demonstrated the effectiveness of non-invasive analyses as a tool to differentiate hands of artists who have worked on the same page. Furthermore, the comparison with analyses carried out on leaves attributed to the workshop of Pacino di Bonaguida allows to investigate in-depth the production of the main illuminators active in Florence at the dawn of the Renaissance.

Determination of lanthanide and actinide elements by energy dispersive x-ray fluorescence spectrometry applying DLLME preconcentration and dried spot

This work describes an analytical procedure to determination of trace amount of lanthanide and actinide chemistry elements (LAEs) in water samples by energy dispersive x-ray fluorescence spectrometry (EDXRF) with the prepare of the samples using simultaneous preconcentration procedure based on the dispersive liquid-liquid microextraction (DLLME). Critical study of the analytical procedure occurred the following way: ions of Eu, Er, Ho, Th, U and Yb presents in 5.0 mL of aqueous sample have been complexed with 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol (Br-PADAP) in a mixture contained solvents (disperser and extractant). After centrifugation, 30 μL of the sedimented organic phase has been removed and deposited on membrane disk and submitted to EDXRF analysis. The optimization step was performed by: i) screening factor with mixture design for the disperser solvent (acetone, acetonitrile and ethanol) and extractant solvent (carbon tetrachloride, trichlorethylene and 1,2-dichloroethane); ii) Box-Behnken design for the independents variables: pH, Br-PADAP concentration, volume of disperser solvent and volume of extractant solvent. The optimized conditions were: 500 μL of disperser solvent (ethanol), 60 μL extractant solvent (carbon tetrachloride and trichlorethylene, 1: 1 ratio), Br-PADAP 1.8 × 10−5 mol L−1 and pH 8.0. In these conditions, the procedure allows the determination of Eu, Ho, Er, Yb, Th and U with quantification limits of 10.5; 8.6; 4.3; 7.0; 6.6 and 1.1 μg L−1, respectively; preconcentration factor between 18 and 74, and precision (RSD%) below that 6%. Salting out effect, presence of other ions, and additions/recoveries of analytes in real samples was verified and the recovery values were between of 90 to 107%. Analytical method has been applied in waters samples and groundwater from uranium mining region.

Study of Potentially Toxic Elements Uptake into Organs of Quercus spp. from Copper Deposits in Slovakia, Italy and Portugal.

The article is focused on the application of Energy dispersive micro X-ray fluorescence spectroscopy as aspecific method to determine the contents of potentially toxic elements and its spread in plant tissues. As a model species, Quercus spp. were selected. In order to compare the obtained results with previous research, four well-described abandoned Cu-deposits were selected for sampling: Ľubietová (Slovakia), Libiola and Caporciano (Italy), andSão Domingos (Portugal). The results of micro X-ray fluorescence spectrometry confirm the irregular contamination of Quercus spp. by potentially toxic elements. The level of contamination is the highest predominantly in the root cortex, where is also the highest Ca contents (with exception of São Domingos). At Ľubietová and Caporciano, high Ni content was described in branches cortex, in branches mesoderm also Fe, Cu and Zn. At the same time, the inhibition influence of Ca was also confirmed regarding the input of these elements into plants.

Composition of inorganic components in <i>Helianthus tuberosus</i> stems

This article studies inorganic components in Heliánthus tuberósus stems. Ash samples and extracts obtained at different pH values were examined. It is established that the extractant's nature has a significant effect on the yield of extractive substances from the ground stems: the greatest (45%) and the minimum (31%) yield was achieved by sodium hydroxide and distilled water, respectively. According to atomic absorption spectrometry, the main ions in the extracts obtained in different media are those of potassium, calcium, sodium, magnesium and iron. Following treatment of stems with solutions having different pH values, the mass fraction of ash varied from 0.4 to 2.3%. The smallest ash yield was observed for a stem sample after acid extraction. According to energy dispersive X-ray fluorescence spectrometry, all ash samples contained predominantly K, Ca, Si and P compounds. Acid hydrolysis produced the highest level of Si in samples, which allows this ash to be used as a silicon-containing material. The ash components of the core and outer part of the stem were compared with the initial sample. According to the nature of thermal decomposition, the initial sample and the outer shell were similar between themselves, though differing from the core. The ash content of the initial sample was 4.3%, with the ash content of the stem core being ~2 times higher than that of the outer shell (7 and 3.8%, respectively). The results of IR spectroscopy showed that splitting of bands in the IR spectra of ash samples depend on the part of the stem and the pre-treatment of raw materials at different pH values. The ash of the initial sample, core and outer shell, as well as the ash of the residues after the aqueous and alkaline hydrolysis of the stem, showed the absorption bands of carbonate groups. The IR spectra of the stem ash after acid extraction contained absorption bands characteristic of amorphous silicon dioxide. According to the conducted X-ray analysis, the studied ash samples were in an amorphous-crystal and crystalline state. The identification of phases was carried out.

Assessment of the Elemental Profile of Leafy Vegetables by Synchrotron-Radiation-Induced Energy Dispersive X-Ray Fluorescence Spectroscopy

Assessment of the Elemental Profile of Leafy Vegetables by Synchrotron-Radiation-Induced Energy Dispersive X-Ray Fluorescence Spectroscopy

ARDESIA-16: a 16-channel SDD-based spectrometer for energy dispersive X-ray fluorescence spectroscopy

We present ARDESIA-16, an X-ray spectrometer based on a monolithic 16-element Silicon Drift Detector (SDD) matrix specifically designed for synchrotron applications. In this work, we describe the main design guidelines which we followed concerning the signal throughput, the energy efficiency, the energy resolution and the overall solid angle covered by detector elements. The characterization of the spectrometer has been made both with radioactive sources in a laboratory environment and with synchrotron light at the P06 beamline (DESY, Hamburg). Experimental results showed an average energy resolution at the optimum peaking time equal to 125 eV (FWHM at Mn Kα), a maximum achieved Output Count Rate (OCR) equal to 17 Mcps, an increase of the energy efficiency above 10 keV thanks to the 1 mm-thick SDD and an overall solid angle equal to 0.4 sr. Finally, we report the first X-ray fluorescence microscopy (XFM) images acquired with an ARDESIA spectrometer.

Variation in the Collimator Beam Size of Energy-Dispersive X-Ray Fluorescence Spectroscopy for Improved Measurement of Gold Purity

Variation in the Collimator Beam Size of Energy-Dispersive X-Ray Fluorescence Spectroscopy for Improved Measurement of Gold Purity

Investigating the Potentials of Sluice Box Angle of Tilt on the Beneficiation of Birnin-Gwari Gold Deposit

The potentials of sluice box angle of tilt on the beneficiation of Birin-Gwari gold deposit was investigated. The sample was sourced from twenty (20) pits on the mine site and homogenized towards chemical characterization. Particle size analysis using 100 g head sample over the sieve range of 500 µm and 45 µm. 100 g each of the homogenized samples was charged into the sluice box at varied tilt angles ranging from 10º to 60º and also at a varying feed rate of 50 kg/hr to 100 kg/hr at 1000 mls flow rate. The Energy Dispersive X-ray Fluorescence Spectrometry (ED-XRFS) revealed 10.15 ppm Au, 0.43% Fe, 0.05% Pb, and other constituent elements in trace form. Particle size analysis showed the liberation size to be -125+90 µm. The highest yield in mass was given as 32.70 g assaying 43.20 ppm at an angle of 10º and varied feed rate while keeping other parameters/constituent constant and also, 56.32 g was the highest yield in mass assaying 12.83 ppm at 50 kg/hr feed rate.Keywords: Birnin-Gwari gold, Beneficiation, Characterization, Sluice box.

Synthesis, crystal structure, and electrochemical hydrogenation of the La2Mg17-xMx (M = Ni, Sn, Sb) solid solutions

The crystal structure of La2Mg17-xSnx solid solution was determined by single crystal X-ray diffraction for the first time. This phase crystallizes in hexagonal symmetry with space group P63/mmc (a = 10.3911(3), c = 10.2702(3) Å, V = 960.36(6) Å3, R1 = 0.0180, wR2 = 0.0443 for the composition La3.65Mg30Sn1.10) and is related to the structure of CeMg10.3 and Th2Ni17-types which are derivative from the CaCu5-type. A series of isotypical solid solutions La2Mg17-xMx (M = Ni, Sn, Sb, x ~0.8) was synthesized and studied by X-ray powder diffraction, energy dispersive X-ray spectroscopy and fluorescent X-ray spectroscopy. All solid solutions crystallize with the structure related to the Th2Ni17-type. The electrochemical hydrogenation confirmed the similar electrochemical behavior of all studied alloys. The amount of deintercalated hydrogen depends on the physical and chemical characteristics of doping elements and increases in the sequence Sn < Mg < Sb < Ni. The most geometrically advantageous sites are octahedral voids 6h of the initial structure, thus a coordination polyhedron for H-atom is an octahedron [HLa2(Mg,M)4].

Heavy metal constituent of medicinal plants: a case study of Moringa oleifera Lam. from selected areas in Accra, Ghana

Background: Anthropogenic activities release metals into the environment that could be absorbed by plants and assimilate into herbal medicines. Objective: This study sought to correlate the outcome of anthropogenic activities that release metals into the environment with levels of metals in medicinal plants using the leaves of Moringa oleifera Lam. (M. oleifera)as a case study. Methods: Leaves of M. oleifera and soil around sampled plants were collected from three locations in the Accra Metropolis: a commercial area, an area with dense vehicular traffic, and a quasi-natural habitat. Samples were analyzed with Energy Dispersive X-ray Fluorescence (ED-XRF) spectroscopy for the presence and levels of arsenic (As), cobalt (Co), chromium (Cr), copper (Cu), nickel (Ni), lead (Pb), vanadium (V) and zinc (Zn). Statistical analyses were performed and the correlation between metal concentrations in leaves and soil was assessed using Spearman’s correlation coefficient. Results: Levels of metals in the leaves and soil samples varied with the site of sample collection. Levels of metals in leaves were significantly lower than permissible limits (p< 0.05) in herbal medicines. Translocation factor (TF) estimates indicated that the M. oleifera leaves exclude the metals under investigation irrespective of the site of collection. However, the TF > 1 in the case of Zn from the quasi-natural habitat signifying bioaccumulation in the leaves. Except forCo, the total concentration of each metal in the soil was not correlated with its concentration in the leaves. Conclusion: The concentration of sampled metals in the leaves and soil varied with the site of sampling and potentially with the anthropogenic activities that release metals into that environment.

Feasibility study on the use of elemental profiles to authenticate aromatic rice: the case of Basmati and Thai rice

Among the thousands of existing rice varieties, aromatic rice has increasingly attracted consumer’s preference in recent years. Within aromatic rice, Basmati, cultivated in some regions in Pakistan and India, is highly demanded. Other aromatic rice, cultivated in specific regions, for instance in Thailand (commonly referred to as Jasmine Thai rice), are also highly appreciated by consumers. In this work, the elemental profiles of commercially available rice samples (17 Basmati, 11 Thai, and 7 Long Grain rice) were determined by energy-dispersive X-ray fluorescence (ED-XRF) spectroscopy. The mass fractions of P, Cl, S, K, Fe, Cu, and Zn were significantly different (95% confidence interval) between Basmati and Thai rice and between Thai and Long Grain rice; only Cl, S, and Zn were significantly different between Basmati and Long Grain rice. Multivariate evaluation of the results combining soft independent modelling by class analogy (SIMCA) and partial least square discriminant analysis (PLS-DA) allowed the correct classification (true positives) of 94.1, 85.6, and 100% of the Basmati, Long Grain, and Thai rice, respectively. The specificity (true negatives) of Basmati, Long Grain, and Thai was 94.4, 82.1, and 100%, respectively.

Investigation of layered double hydroxide/carbon dot nanocomposite on removal efficiency of Pb2+ from aqueous solution

In this study, double layered hydroxide (LDH)/carbon dot (C-dot) nanocomposite was synthesized using coprecipitation and hydrothermal methods, respectively, and used to remove Pb2+ ions from water. The chemical composition and morphology of the Mg-Al LDH/C-dot nanocomposite structure were investigated by Fourier transform infrared spectroscopy (FT-IR), x-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and fluorescence spectroscopy (FS). Batch adsorption was accomplished to evaluate the process of Pb2+ adsorption by Mg-Al LDH/C-dot nanocomposite. For this purpose, parameters were optimized such as pH, C-dot to Mg-Al LDH ratio, adsorbent dosage, and contact time. The value obtained are 7, 0.25, 16 mg and 40 min, respectively. The results showed that the adsorption of Pb2+ on the Mg-Al LDH/C-dot nanocomposite has a maximum adsorption capacity of 41.32 (mg.g−1), which can be attributed to the available presence of functional groups. The adsorbent performance was investigated by the Langmuir, Freundlich and Dubinin-Radushkevich isotherms and the pseudo-first-order and pseudo-second-order kinetic models, respectively. Adsorption isotherm followed the Langmuir equation, that demonstrate monolayer adsorption and the pseudo-second-order kinetic model shows that a chemical adsorption controls the reaction rate. According to the results, the Mg-Al LDH/C-dot nanocomposite can be considered as an efficient adsorbent for the adsorption of Pb2+ ion from aqueous solution.