EDXRF Spectrometer Research Articles

Seasonal and Spatial Variations in Particulate Matter, Black Carbon and Metals in Delhi, India’s Megacity

This study explores the spatial patterns of particulate matter (PM) in the megacity of Delhi. A GRIMM aerosol spectrometer is used to analyze different aerodynamic diameters (PM10, PM2.5, PM1.0), inhalable, thoracic, and alveolic particles, and black carbon (BC) at six prominent locations in Delhi during summer and winter. Additionally, metals (Pb, Fe, Ca, Al, Zn), along with silicon and sulfur, are analyzed using an ED-XRF spectrometer over the sampling locations during the summer season. The sampling site data are interpolated using the Kriging method to generate spatial maps to explore the air pollution problem in Delhi. East Delhi is observed to be the most polluted site, while Guru Gobind Singh Indraprastha University (GGSIPU) is the least polluted site. We further observe a high correlation between Al-Fe, Al-Ca, Zn-Pb, Ca-Fe, and S-Zn, indicating their common source of emission. Aerosols are also found to be highly enriched with metals like Al, S, Fe, Zn, and Pb, suggesting strong anthropogenic sources of these metals. Construction activities, resuspended dust, an increased number of vehicles, faulty agricultural practices, and soil could be recognized as major sources of the particulate concentration in an urban area like Delhi.

Study of chemical effects on L X-rays spectra of 59Pr compounds using high resolution WDXRF and EDXRF measurements

Chemical effects on L X-rays spectra of PrF3, PrCl3, PrBr3, Pr2O3, Pr6O11 and Pr2(SO4)3 compounds have been investigated from measured ILi/ILα (i = l and β6), ILj/ILβ1 (j = η, γ5 and γ1), ILk/ILγ1 (k = γ5 and η) intensity ratios using high resolution poly-chromatic WDXRF, and monochromatic excitation by 6.49 keV in vacuum (10−2 Torr) and Ag Kαβ (22.581 keV) X-rays photons in EDXRF spectrometers. The experimental results clearly exhibit significant variation in measured intensity ratios of L X-ray components of investigated compounds from pure elemental form and theoretically predicted values evaluated using different atomic parameters. Furthermore, the change in inner shell/subshells binding energy resulting from the transitions of outer shell/subshell electrons is also inferred from the shifts of order ∼0.1–0.70 eV in Ll, Lβ2 and Lγ1 components of PrF3, PrCl3, PrBr3, Pr2O3, Pr6O11 and Pr2(SO4)3 WDXRF spectra relative to pure 59Pr. The variation in intensity ratios and shift in Ll, Lβ2 and Lγ1 X-ray components of 59Pr compounds are attributed to crystal defects, structural effects and exchange interactions between core and valence electrons of different ligands attached to central 59Pr atom. The reliable experimental data would be helpful in the theoretical interpretation of standard reference data for inner-shell vacancy decay parameters used in X-ray fluorescence analysis of compound samples.

Analysis of cultural heritage reference materials by portable and energy dispersive X-ray fluorescence measuring methods: results reliability assessment

This article discusses the results of a large-scale analysis of five cultural heritage alloy reference materials (CHARM) and their shavings using handheld (pXRF) and stationary energy dispersive (ED-XRF) spectrometers. The primary objective of these studies was to assess the capability of the pXRF and ED-XRF spectrometers as a non-invasive surface-measuring technique used for the analysis of the reference materials and the reliability of the data obtained. The second objective was to evaluate the capability of the pXRF and ED-XRF spectrometers used for the analysis of shavings of the same five reference materials and to assess the data obtained. These objectives required finding the best fitting analytical tools for the comparison, and the assessment of the reliability of the data, and, very importantly, finding reliable models for data analysis and results validity verification. Based on the analysis carried out on the cultural heritage alloy reference materials, it can be concluded that the results of XRF spectrometry obtained from both spectrometers are reliable and can be compared to each other by making reference to four basic conditions: that the provided analysis should be based on certified reference materials of known elemental composition; that analysis be performed according to appropriate measuring methodology (research protocol); that analysing tools (predictive analytics) be clearly defined; and, finally, that testing be done on archaeological artefacts. The reliability and inter-correlation of the results obtained were assessed to determine the possibility of successfully applying XRF spectrometry in the investigation of archaeological artefacts produced from copper alloys.

Analysis of the Characteristics of Heavy Metal Elements in Soil Around the Smelting Area of Pasuruan Industrial Estate, Indonesia

Abstract Smelting plant is an activity that produces emissions in the form of heavy metal particulates that can cause pollution and are harmful to human health in excessive concentrations. This research was conducted to determine the heavy metals’ characteristics in the soil around the metal smelting area of Beji industrial area, Pasuruan, Indonesia. A total of 33 soil samples were collected at 200 m, 500 m, 2km and 5km from the metal smelting area. The concentrations of heavy metals Zn (669.47 - 63.25 mg/kg), Cd (94.88 - 40.30 mg/kg) and V (198.98 - 108.19 mg/kg) in the soil were determined by using EDXRF Spectrometer Minipal 4. The concentration of zinc reduces with distance from an industrial region. The amounts of cadmium and vanadium did not change considerably with distance. Then the potential pollution risks of heavy metal in the soil were evaluated by method of assessment of heavy metal contaminations in soil. These Cf values indicated that the assessment of heavy metal contamination in soils from smelters was category: Indicates no contamination, suspected contamination, slight contamination and extreme contamination.

Experimental Investigation of gamma-ray shielding capability of clay used as building materials in Thi Qar Province

Clay is one of the oldest building materials known to man uses in construction. This material has many important potentials and features, and the methods of using this material in construction in the past and present varied greatly, responding to environmental determinants; Such as the climate, the quality of the soil, and the available materials on the one hand. The aim of the present study is to test the ability of this material to attenuate gamma-ray radiation. Gamma ray attenuation coefficients such as linear and mass attenuation half value layer, tenth value layer, and mean free path for deferent thickness slabs of clay was measured using 3”×3” NaI(Tl) gamma spectroscopy system at energy 662 KeV, 1173 KeV, and 1332 KeV. The measured values of the attenuation parameters showed good agreement with the theoretical calculations. The elemental compositions of the clay slabs analyzed by using an EDXRF spectrometer. The obtained results appear that the clay is a suitable alternative for radiation protection and achieve a safe level of radiation exposure for photons that have moderate energy.

Study on the pigments of Chinese architectural colored drawings in the Altar of Agriculture (Beijing, China) by portable Raman spectroscopy and ED-XRF spectrometers

The in-situ measurement was carried out on the pigments used in the colored drawings in the Altar of Agriculture (Beijing, China) for the first time by portable Raman and ED-XRF spectrometers. Three kinds of colored drawings (the original drawing, the restored drawing, and the repainted drawing) located in Sacrificial Storehouse were studied. The information of the pigments, including red lead, white lead, indigo, carbon black, and atacamite were found in the original drawing, while Bright red β-naphthol, Sudan Ⅰ, chrome yellow, titanium dioxide, ultramarine blue, and phthalocyanine green were identified from the repainted drawing. Chrome yellow, ultramarine blue, and phthalocyanine green were used in the green and blue regions of the restored drawing. According to the application history of the pigments and the records of the Altar of Agriculture, the original colored drawing could be dated to the Qianlong period. The pigments used in restoration and repaint hadn’t followed up the original drawing. The main reason is a lack of knowledge about the pigments used in the original painting. Hence, the information of the pigments used in these original drawings is of great guiding significance for the subsequent protection and restoration of the architectural drawings in Altar of Agriculture (Beijing, China).

Handheld ED-XRF spectrometers in geochemical investigation: Comparative studies for glacial deposits from Spitsbergen

Handheld ED-XRF spectrometers in geochemical investigation: Comparative studies for glacial deposits from Spitsbergen

Reconstruction of metal(loid)s pollution history in sediments of Wami Estuary, Indian Ocean Coast of Tanzania

Results of metal(loid)s pollution history, their enrichment and contamination factors in sediments of Wami River Estuary, Tanzania are presented. Two sediment cores (WE1 and WE2) were retrieved from the Estuary using hand-driven PVC coring tubes. Levels of metal(loid)s in sediment samples were determined using EDXRF spectrometer coupled with X-lab ProTM software. Metal(loid)s enrichment factors (EF) were determined using metal(loid)s baseline values established during this study. Contamination factors were determined by dividing measured metal(lod)s concentrations in the samples by their respective baseline concentrations. Sediment physical chemical parameters were determined in order to establish their relationship with metal(loid)s concentrations. Sediment chronologies were established using the Constant Initial Concentration (CIC) lead-210 sediment-dating model in order to convert sediment depth profile into timescales. The lowest concentrations of As in sediments was measured in sediments deposited during 1960s, followed by increase reaching the highest concentrations in sediments deposited between ca. 2015 and 2017. Lowest and highest concentrations of Cd were measured in 1960’s and ca. 2000, respectively. Cu and Zn had their maximum concentrations in ca. 1971 and their significant positive correlation (r = 0.94, p = 0.01) suggest common origin of these metals. Average metals enrichment factors in the core were established and are in the order As = Cd = Cu = Pb = Zn = 0.1. This EF value suggests that all metals in sediments of Wami originate from natural sources (EF < 1). Metal(loid)s contamination factors (CF) were low to moderate for As, Cu and Zn; moderate for Pb; and low to considerable for Cd. CIC model revealed that the sediment at the bottom of cores WE1 and WE2 date back about 33 and 55 years, respectively. Sediments of Wami Estuary is characterized by mixing as evidenced in the established chronologies. Therefore, reported radiometric dates should be considered as a preliminary chronological estimate and further research is needed focused on terrestrial records of anthropogenic activities.

Computational screening of trace elemental concentrations in Hemidesmus indicus L. A potential herbal plant used against skin diseases by ED-XRF-Technique

The present investigation reports on the screening of 13 trace elemental concentrations in the leaves of Hemidesmus indicus, an anti-skin disease medicinal plant of Telangana by ED-XRF technique. ED-XRF spectrometer is a non destructive, multi-elemental capability, excellent sensitivity and low detection limits for large atomic numbers. The elements like P, Cl, S, K, Mn, Ca, Cu, Fe, Se, Br, Zn, Sr, and Rb were identified and its concentration determined. From the present results the concentration of Cl, Ca, Mn, Fe, Cu, Zn Se, Rb, Sr and Br were found at a higher level while the concentration of P, S and K identified at minor level compared with NIST 1515 apple leaf. Present data indicate that, the safe use of this herbal plant leaves in the conventional treatment of skin disorders because this medicinal plant leaves are contain substantial quantity of Mn, Fe, Cu, Zn, and Se.

Quantitative X-ray fluorescence analysis: Trace level detection of toxic elemental impurities in drug product by ED-XRF spectrometer

Inorganic impurity analysis of pharmaceutical drug products is of paramount importance at trace levels due to the availability of toxic metals. The existing techniques require extensive development and chemical treatment to evaluate the presence of class I (Pb, Cd, Hg and As) and class II (Co, V and Ni) heavy metal elements which are harmful to the environment. To overcome these issues, a cost and time effective wavelength dispersive X-ray fluorescence spectrometry (XRF) was introduced to determine the concentration of trace elements in one of the angiotensin receptor blocker (ARB) (tablet sample 300 mg) according to guidelines addressed in ICH Q3D and USP. The validation study focused on class I and class II elements are also in accordance with regulatory guidelines. Overall it includes the comprehensive characterization of analytical method which is compliant with the requirement of USP. The novelty of this work includes the application of EDXRF in routine analysis of trace elements (especially volatile Hg) present in the pharmaceutical product beyond the previously published studies for the limited number of the non-pharmaceutical regime. Apart from this it also requires minimal sample preparation and method development and is able to quantify toxic impurities which are present in the sample in less than 20 ppm concentration, with the lowest level of detection up to 0.1 ppm.

ED-XRF: a promising method for accurate and rapid quantification of metals in a bacterial matrix

ABSTRACT The remediation of metal-polluted water using bacterial biofilms is a promising technology. In order to help its development, the present study aims to evaluate the feasibility to utilize XRF spectrometry for accurate and rapid measurement of metal concentrations in bacterial biofilms used in treatment plants. For that purpose, an ED-XRF spectrometer was used to measure Cd, Cu, Fe, Mn, Ni and Zn concentrations within a matrix of marine bacteria Pseudomonas fluorescens BA3SM1 and its metabolites. Contaminated and control cultures of the strain BA3SM1 were dried and crushed, then analysed by ED-XRF. The LOD value of the analysed metals was between 2.08 and 10.5 µg g−1. Metal concentrations were also measured by ICP-AES or ICP-MS to support ED-XRF results. The two techniques showed a good linear correlation with a slope of at least 0.949 and R 2 of at least 0.985. These results confirm the possibility to measure metal contents by ED-XRF in bacterial matrices.

Environmental assessment of heavy metal pollutants in soils and water from Ortum, Kenya.

Analysis of elemental concentration in soil and water was carried out in Ortum to ensure safe utilization of soil and water resources for agriculture, industrial, and household purposes. Elemental analysis of soil and water was done using the EDXRF spectrometer and the inductively coupled plasma - optical emission spectrometry (ICP-OES), respectively. A total of 59 soil samples from different locations and depth and 10 water samples were collected from Ortum using purposive sampling method. The results of the mean elemental composition of 13 elements Ni (ppm), Cu (ppm), Zn (ppm), Pb (ppm), K (%w), Ca (%w), Fe (%w), Ti (%w), Mn (ppm), Rb (ppm), Sr (ppm), Zr (ppm), and Nb (ppm) in soils were 58.11, 46.91, 73.49, 22.20, 3.83, 24.39, 1.72, 7.73, 1529.74, 60.98, 442.26, 410.63, and 29.36, respectively, and the mean of 19 elements Ni, Cu, Pb, Zn, Ag, Al, As, Ba, Ca, Cd, Co, Cr, Fe, K, Mg, Mn, Mo, Na, and Se in water samples in (mg/l) were 0.037, 0.0014, 0.0005, 0.0042, 0.0030, 0.021, 0.0080, 0.12, 73.81, 0.00023, 0.0036, 0.00276, 0.0040, 6.11, 38.18, 0.00023, 0.0032, 46.87, and 0.0026, respectively. The average elemental concentration in soils was within the world average range. The mean concentration of Cu, Zn, and Pb in soil reduced with increase in depth while that of Ni increased with increase in depth. The average metal pollution indices in soils, geoaccumulation index (Igeo) potential ecological risk index (Ei), and synthesized potential ecological risk index (Er) were evaluated and found to be - 0.40, 4.92, and 19.69, respectively. According to the classification index, the results show that the soil in Ortum is moderately polluted, and the risk associated with the measured elemental concentration of Ni, Zn, Cu, and Pb in the soils is low. The elemental concentrations in water sampleswas lower than the recommended permissible limits except for Calcium (Ca) in borehole water with an average of 90.80mg/l against the permissible levels of 75mg/l(WHO, 2011). The pH for water samples was found to range from 6.60 to 7.71 with an average of 7.07 which is within the acceptable range of pH6.5 to pH8.5 as recommended by WHO, 2011.The study found out that elemental concentration in soil and water samples from Ortum were withing the world average values and that the soil and water in Ortum is safe for use in agriculture and domestic purposes.

Determination of Seasonal Variation of Air Pollution in Rize Province by Using a Type of Biomonitor Moss Hypnum cupressiforme

In this study, in order to determine the level of seasonal heavy metal pollution in Rize province, by placing Hypnum cupresiforme (a species of moss) samples into twelwe stations, Cr, Fe, Ni, Cu, Pb and Al concentrations were determined by using EDXRF Spectrometer (Epsilon 5, PANanalytical). The mean concentrations of Cr, Fe, Ni, Cu, Pb and Al were found to be 9.5 µg.g-1, 2370 µg.g-1, 5.4 µg.g-1, 15.9 µg.g-1, 5.3 µg.g-1 and 3712 µg.g-1, respectively. These levels were compared to mean values obtained from the other studies in Turkey. In this study, Al value was higher than the mean values obtained from the national studies, whereas Cr, Fe, Ni, Cu and Pb values were found to be lower. In addition, the results obtained from this study were compared with the permissible heavy metal limits for the plants by international organisations.

Evaluation of full‐field energy dispersive X‐ray fluorescence imaging apparatus and super resolution analysis with compressed sensing technique

A full‐field energy dispersive X‐ray fluorescence (FF‐EDXRF) imaging spectrometer that utilizes single‐photon counting analysis with a charge‐coupled device was developed in our laboratory.We evaluated the developed spectrometer with respect to its energy resolution, spatial resolution, quantitative performance, and elemental imaging and compared it with the corresponding characteristics of scanning‐type EDXRF spectrometers. In addition, we demonstrate that the limit of detection and sensitivity deteriorate as the analytical area decreases. Finally, compressed sensing, which is a widely used information‐processing technique, was applied for clearing XRF images.

Investigation on Li (i = l, β, and γ)–to-Lα X-ray Intensity Ratios of Tl in Thallium Compounds

The Li(i = l, β, and γ)–to-Lα X-ray intensity ratios of Tl in some thallium compounds were measured by EDXRF spectrometer. These compounds were excited by 59.5 keV gamma-rays from a 241Am annular radioactive source. L X-rays emitted by the compounds were counted using an Ultra-LEGe detector with a resolution of 150 eV at 5.9 keV. Li–to-Lα X-ray intensity ratios of Tl in these compounds are compared with that of the pure Tl calculated theoretically. While the values of Ll/Lα and Lγ/Lα intensity ratios are compatible with the theoretically calculated value, the values of Lβ/Lα intensity ratios have differences.

Environmental Pollution by Heavy Metals in the Gold Mining Region of East Cameroon

The main objective of this study is to assess the level of heavy metals pollution in soil samples collected around gold mines located in Betar&eacute; Oya (BO) and Batouri (BA) in Eastern Cameroon. Elemental analysis of soil samples was carried out using Quant´X EDXRF spectrometer. Its sensitivity and accuracy were increased by using the Fundamental Parameter approach for quantification of the results. Analysis results showed high content of iron (39300±200 ppm), the presence of manganese (730±70 ppm), arsenic (4±2 ppm), zirconium (314±4 ppm) and lead (79±9 ppm) as compared to worldwide average upper continental crust (UCC). The mean Enrichment Factors (EF) decrease as Pb>As>Zr>Mn>Fe>Y>Ga>Zn>Cu>Ni> Rb>Sr>Sn>Ba in agreement with the Contamination Factors (CF). The values of pollution load index (PLI) were found to be low in all the studied samples and indicate that the studied sites in Bétaré Oya and Batouri are in low pollution status regarding the total of the studied metals. Results of this study pointed out that soils examined in the gold mining areas of Eastern Cameroon are polluted by heavy metals. It is therefore important that measures should be geared towards strengthening the monitoring of mining areas to stem down the level of contamination of soil. Phytoremediation of sites after closing open pits or the biogeosystem method would be a suitable way of regulation of the studies areas.

Determination of Heavy elements in Drinking Water from Different Regions of Baghdad City (Iraq) Using EDXRF Spectrometer

It was calculated the average concentrations of elements manganese, iron, cobalt, nickel, copper, zinc, arsenic, cadmium and lead in the sixteen samples of drinking water (tap water), were collected from different areas in the Baghdad city. The Results indicated that the average of concentrations of the elements Mn, Fe, Pb, Ni and Cd (0.44ppm, 0.49ppm, 0.04ppm, 0.17ppm and 1.2ppm respectively) higher than permissible limit while the concentrations of elements Cu and Zn (0.11ppm and 0.14ppm respectively) were lower than the permissible limit of World Health Organization (WHO) standards (1ppm and 3ppm) respectively for drinking water and the concentration of Arsenic in the nuclear lab sample in college of sciences - Mustansiriyah University was higher than permissible limit. &#x0D; All the drinking water samples were analyzed and determined the physical and chemical properties such as Electrical Conductivity (EC), pH, and Total Dissolved Solids (TDS). The highest value was (1064μS/cm) in Al-Tuwaitha sample and the lowest value (531μS/cm) in Al-Sadr City (Sector 7) sample for the Electrical Conductivity. The pH values ranged from (7.0-8.2). The average levels of Total Dissolved Solids (TDS), the highest value was 550 mg/L in the Diyala Bridge sample while the lowest value 276mg/L in Al-Sadr City (Sector 7) sample. The results were compared with national and international standards, and it’s also showed that the values of the parameters within the permissible limit of World Health Organization (WHO) standards, except the Electrical Conductivity values for some samples were higher than permissible limit. According to these results, all the water projects must be monitored as well as using the proper and modern techniques for treatment the drinking water.

Comparison of PIXE and XRF analysis of airborne particulate matter samples collected on Teflon and quartz fibre filters

Abstract Within the framework of research projects focusing on the sampling and analysis of airborne particulate matter, Particle Induced X-ray Emission (PIXE) and Energy Dispersive X-ray Fluorescence (ED-XRF) techniques are routinely used in many laboratories throughout the world to determine the elemental concentration of the particulate matter samples. In this work an inter-laboratory comparison of the results obtained from analysing several samples (collected on both Teflon and quartz fibre filters) using both techniques is presented. The samples were analysed by PIXE (in Florence, at the 3 MV Tandetron accelerator of INFN-LABEC laboratory) and by XRF (in Elche, using the ARL Quant’X EDXRF spectrometer with specific conditions optimized for specific groups of elements). The results from the two sets of measurements are in good agreement for all the analysed samples, thus validating the use of the ARL Quant’X EDXRF spectrometer and the selected measurement protocol for the analysis of aerosol samples. Moreover, thanks to the comparison of PIXE and XRF results on Teflon and quartz fibre filters, possible self-absorption effects due to the penetration of the aerosol particles inside the quartz fibre-filters were quantified.

Contextualizing Bronze Age Obsidian Use at the ‘Ritual Spring’ of Mitza Pidighi (Sardinia)

This study focuses on obsidian consumption at the ‘ritual spring’ of Mitza Pidighi in west-central Sardinia, Italy. The site dates to the late Nuragic I to Nuragic III phases of the Bronze Age (ca. 1350–850 B.C.) and is found just east of a contemporaneous residential village, Nuraghe Pidighi. While recent years have seen a surge of archaeological literature on the subject of obsidian use at residential sites throughout the island, there has been little consideration of its role in other archaeological contexts, a research bias that this presentation aims in part to redress.For this study, 142 obsidian artifacts from Mitza Pidighi were analyzed non-destructively using a Thermo Scientific ARL Quant'X EDXRF spectrometer to determine their geological origins. In addition, each artifact was analyzed techno-typologically to allow for the reconstruction of the entire chain of events leading up to an artifact's discard. The sourcing results show that obsidians from all four Sardinian subsources are represented at the site, although most come from just one outcrop; the typological analysis indicates that people were physically knapping obsidian near the well to create expedient flake tools and non-prismatic bladelets. In combination, these results have important implications for interpreting the social, economic, and symbolic function of Mitza Pidighi and in understanding the role of obsidian outside of domestic contexts.

Effect of Long-time X-ray Irradiation on Cr and Hg in a Polypropylene Disk Certified Reference Material Observed during Measurements by X-ray Fluorescence Spectrometry.

The effect of long-time X-ray irradiation on Cr and Hg in a polypropylene disk certified reference material (PP disk CRM, NMIJ CRM 8136-a) during measurements by X-ray fluorescence (XRF) spectrometry was examined in the present study. The XRF intensities of Cr (Kα), Hg (Lα) and Pb (Lα), obtained by an energy-dispersive (ED)-XRF spectrometer, showed the different intensity trends and the obtained XRF intensity ratios of Cr/Pb and Hg/Pb revealed decreasing and constant ratios, respectively, for long-time X-ray irradiation of up to 430 h. A similar decreasing trend of the Cr/Pb intensity ratio was also observed by wavelength-dispersive (WD)-XRF measurements for 120 h. Moreover, Cr, Hg and Pb in the PP disks obtained after long-time measurements by the WD-XRF spectrometer were measured by an ED-XRF spectrometer, and the loss of Cr was confirmed. From these results, Cr in the PP disk CRM, whose chemical form was an organometallic compound, was considered to be possibly lost during the XRF analysis for long-time or frequent measurements.