Energy Dispersive X-ray Fluorescence Research Articles

The Use of Energy Dispersive X-Ray Florescence to Evaluate Some Heavy Metals as Pollutants in <i>Heterotis niloticus</i> and Sediment from Baga, Lake Chad, Nigerian Sector

The pollution of aquatic ecosystems by heavy metals is a major global concern, presenting significant environmental and health hazards. This research evaluated the concentrations of Cd, Cr, Cu, Pb, and Zn in H. niloticus and sediments from Dumba 1, Baga, Lake Chad, Nigerian Sector using energy dispersive X-ray fluorescence (EDXRF). The results indicated high concentrations of Cd, Cr, Cu, and Pb (0.45 ± 0.01, 2.14 ± 0.03, 14.46 ± 0.25, and 6.38 ± 0.05 mg/kg), which are higher than the maximum acceptable limits set by World Health Organization (WHO). The findings suggest contamination of H. niloticus by these heavy metals (Cd, Cr, Cu, and Pb), highlighting potential health risks. Additionally, sediment analysis showed concentrations of Cd, Pb, and Zn (2.62 ± 0.1, 120.15 ± 5.01, and 102.67 ± 6.02 mg/kg) exceeding acceptable limits for average shale, indicating sediment contamination and possible environmental health risks to both fish and humans.

Energy Dispersive X-ray Fluorescence for Elemental Analysis of Foods

Energy Dispersive X-ray Fluorescence for Elemental Analysis of Foods

A Case of Identity: A Technical Study of Victorian Wallpapers

ABSTRACT Public perception of arsenic in nineteenth-century Britain encompassed a variety of things: criminal poison, useful medicine, and a raw material for manufacturing an array of goods. During this era, Henry Carr tested wallpaper and fabric samples sent in by private individuals and manufacturers, as part of an early effort in gathering scientific data to inform and protect consumers against chronic arsenic poisoning. In 2022, eight wallpaper samples that Carr had tested were acquired by Winterthur Library. These samples were analyzed by polarized light microscopy, scanning electron microscopy with energy dispersive X-ray spectroscopy, X-ray fluorescence, and Raman spectroscopy to identify the presence of arsenic. Of the eight wallpaper swatches, seven suggested trace-to-elevated levels of both arsenic and copper. Two swatches were confirmed as having the arsenical pigment emerald green (copper acetoarsenite) specifically. Research into these wallpaper samples furthers the legacy of knowledge gathering and sharing in order to protect everyday users by contributing to toxicology research in library and archives materials.

Determination and Removal of Potentially Toxic Elements by Phragmites australis (Cav.) Trin. ex Steud. (Poaceae) in the Valles River, San Luis Potosí (Central Mexico)

The contamination of rivers by potentially toxic elements (PTEs) is a problem of global importance. The Valles River is Ciudad Valles’ (Central Mexico) main source of drinking water. During the four seasons of the year, water samples (n = 6), sediment samples (n = 6), and Phragmites australis plants (n = 10) were taken from three study sites selected based on the presence of anthropogenic activities in the Valles River. A graphite atomic absorption spectrophotometer estimated elements in the water, and an energy-dispersive X-ray fluorescence spectrometer quantified elements in sediments and plant samples. Phragmites australis accumulated metal(loid)s mainly in the roots during all seasons of the year. Water samples from all sites recorded PTEs (As, Pb, Cd, and Hg), with primary sources identified as the sugar industry, urban and industrial wastewater, and the combustion of fossil fuels. Sediment samples showed concentrations of Hg, Mn, Ni, Zn, Pb, V, Cu, Cr, and Cd, attributed to agricultural practices, industrial activity, and urbanization. P. australis is an alternative for in situ phytoremediation because this macrophyte can bioaccumulate different elements in its roots, such as Mn, Rb, V, Sr, Cu, Zn, Pb, Ni, and As.

Scientific research on white potteries from the Nanzuo site in Qingyang, Gansu province

AbstractLocated in Qingyang, Gansu province, China, the Nanzuo site on the Loess Plateau is a large‐scale, high‐ranking central settlement of the late Yangshao period with capital city characteristics. We used a thermal dilatometer, energy‐dispersive X‐ray fluorescence (EDXRF), optical microscope, scanning electron microscopy with energy‐dispersive spectroscopy (SEM‐EDS), X‐ray diffraction (XRD) and Raman spectrometer to analyse the firing temperature, composition, microstructure and phase composition of the white potteries in the Nanzuo site. The results indicate that kaolin, china stone and local fusible white clay are the raw materials of the body. The surface coatings of white potteries are formed from shells. The main constituents that make up the internal surface coating are aragonite and calcite, which are derived from the prismatic and nacreous layers of shells. The external surface coating is composed of CaCO3 nanoparticles that arrange themselves as aragonite tablets within the nacreous layer. This exceptional pottery‐making technique is exclusive to Nanzuo and has not been reported at any other site in the world. This technique is significant for researchers to deepen our understanding of pottery‐making technology history in China.

Seasonal and Spatial Discrimination of Sandy Beaches Using Energy-Dispersive X-Ray Fluorescence Spectroscopy Analysis: A Comparative Study of Maltese Bays

The general increase in awareness of environmental pollutants and typical sources reflects the application of sustainability and development goals. Energy-Dispersive X-Ray Fluorescence spectroscopy analysis has been used to analyse sand samples collected from five different beaches located on the east and north-eastern coasts of Malta and Gozo during two summers and two winters. Samples were collected along linear transects perpendicular to the shoreline at three different depths. Chemometrics were used to discriminate between four latent variables, including season, location, depth, and distance from shoreline. The highest concentrations were attributed to Fe2O3, Al2O3, SrO, and SnO2. Principal Components Analysis and Factor Analysis classified distributions of Fe2O3, CoO, As2O3, MnO, SrO, SeO2, and CaCO3 under Principal Component 1. However, since no loading value dominance was observed, such distributions most likely represent a combination of lithogenic and anthropogenic natures. Discrimination using Stepwise Linear Canonical Discriminant Analysis (SLC-DA) and Partial Least Squares Discriminant Analysis (PLS-DA) using Leave-One-Out-Cross-Validation with Variance Importance Plots proved highly effective in classifying data by location, followed by seasonal variability. It follows that concentrations are not affected by depth and distance from shoreline variability, proving that accumulation and anthropogenic effects from land are not concentrated in specific zones but are spatially spread out along the bays and do not increase with depth.

From copper‐based alloys to coins—Part I: Metallurgical characterization from complex manufacturing processes of imitation coins dated to the third century CE

AbstractThe evidence for imitation coinage found on the Gallo‐Roman site of Châteaubleau (Seine‐et‐Marne, France) has been attested for several years. Successive excavations and findings related to the production of imitation coins, both struck and cast, have revealed major minting activity during the second half of the third century CE. This paper presents the study of 11 archaeological samples issued from this counterfeiting workshop site, which is today considered the most important in the north‐western provinces of the Roman Empire. These samples, which correspond to different stages in the production chains leading to coins, mainly radiates (antoniniani, double sestertii), were characterized by metallography, energy‐dispersive X‐ray fluorescence (EDXRF), scanning electron microscopy with energy‐dispersive spectroscopy (SEM‐EDS) and the Vickers hardness test, in order to understand the different manufacturing processes, especially the ‘rod to coin’ one. This project is divided into two parts. The first, which is the subject of this paper, focuses on the chemical and metallurgical study of the archaeological artefacts. This has enabled us to identify and characterize the manufacturing processes thanks to the highly characteristic microstructure of the samples from the rod‐to‐coins process. Some of the cylinders derived from this process were also silvered by plating a foil of silver or silver–copper on a flan of pure copper in order to obtain irregular radiates. As regards fake double sestertii, several manufacturing techniques were identified: direct moulding of coins in stacked terracotta moulds, the casting of flans to strike double sestertius and the cutting of flans from metal plate is also a technique used in Châteaubleau. Characteristic composition and microstructures were also observed in these samples. This paper will be followed by a second focused on two experimental archaeology sessions carried out in order to reproduce the process ‘from rod to coins’ and then to compare the reproduced samples with the archaeological samples.

Geochemical Profiles of Deep Sediment Layers from the Kolubara District (Western Serbia): Contamination Status and Associated Risks of Heavy Metals

Global awareness of the harmful effects of heavy metal contamination in soil has increased significantly. Understanding the vertical distribution of oxides and elements is vital for tracing the history of potential contamination. Thus, this study focuses on deep sediment cores primarily composed of quartz and clay minerals from a small village in the western Tamnava Basin of Serbia. The aim was to assess the vertical distribution of 11 oxides and 21 elements and the ecological risks of eight heavy metals by analyzing 250 sediment samples from 18 boreholes at depths ranging from 5 to 58.5 m. Deep sediment core samples were analyzed using energy-dispersive X-ray fluorescence spectrometry (ED-XRF). Potential contamination levels were evaluated within the study area. Additionally, samples were analyzed for total carbonate and organic carbon contents and particles retained on a 0.063 mm sieve. Higher than permitted concentrations of vanadium (V), thallium (Tl), and barium (Ba) were found. Notably, this zone is located above a proposed lithium and boron mine in Gornje Nedeljice, making it crucial for monitoring efforts. Even if mining operations do not commence, examining the deep sediment layers in this rural area remains important. This study offers novel and valuable data on the concentrations of potentially toxic elements in undisturbed deep sediment, serving as a benchmark for future comparisons.

Influence of road surface type on the magnetic susceptibility and elemental composition of road dust

The aim of the study was to determine the effect of the type of road surface (asphalt and concrete) and the presence of noise barriers (acoustic screens) on the magnetic susceptibility and chemical composition of road dust collected from national roads and motorways in central and southern Poland. Four roads with asphalt surfaces and four with concrete surfaces were selected for the study. Samples were taken at three control points: in the space between noise barriers, in the space without barriers and at road exits. Magnetic susceptibility measurements and elemental composition analysis (using an energy dispersive X-ray fluorescence spectrometer) were carried out. The results showed high variability with no clear differences between samples taken from asphalt and concrete roads. Magnetic susceptibility values were higher for road dust taken from asphalt pavements near noise barriers and motorway exits, while for open space samples the susceptibility values were about 1.3 times higher for dust from concrete pavements. A similar relationship was observed for the elemental composition. The results showed no clear differences between samples taken from asphalt and concrete roads. The location of the sampling point had a greater influence on the results: the surface of noise barriers, open spaces or motorway exits. Calculated enrichment factors indicated an extremely high enrichment of dust in elements such as Cr, Cu and Zn, a very high enrichment in Pb only for dust collected at motorway exits, and a significant and moderate enrichment in other elements.

Some educational uses of EDXRF for technologists in health science

Abstract Physicists teach physics to students of various academic disciplines such as physics, chemistry, health sciences, biology, geology, environmental sciences, etc. Energy dispersive x-ray fluorescence spectroscopy (EDXRF) is a case of application of atomic physics in the real world. Students, through applications of EDXRF, may find out how the basic concepts of atomic physics can be used for elemental analysis of samples of their scientific interest and everyday life. This paper presents some educational implementations of EDXRF and highlights the importance of incorporating this spectroscopic method in undergraduate or postgraduate labs or lectures in the field of health sciences. Five experimental activities, a general one for understanding x-ray spectra and the others for the analysis of substances/materials related to chemistry/toxicology, dentistry, optics, and cosmetics, are presented and discussed.

Determination of Trace Metal Composition in Ambient Air from Open Burning of Solid Waste in Aiyekale, Nigeria

Open burning of solid municipal waste uncontrolledly presents an environmental menace, which exacerbate air pollution and poses considerable health risks in most developing countries. This study aims at investigating the seasonal deposition fluxes, trace metal concentrations and determination of scavenging ratios of the identified metals, resulting from such practice in Aiyekale, Kwara State, Nigeria. The particulate matter of both dry and wet samples was collected using deposition gauges. The elemental composition of particulates collected was analyzed using Energy-Dispersive X-ray Fluorescence Spectroscopy (EDX-RF). The deposition velocity and scavenging ratio were used to study the removal mechanics of trace metal composition of the ambient air in open burning of solid waste area. The average flux rate in the wet and dry seasons was evaluated to be 3.57 × 10-6 g/m2.s, and 2.28 × 10-5 g/m2.s, respectively. For the study area, the deposition velocities for the trace metals ranged from 5.288 × 10-5 to 4.818 × 10-3 m/s while the estimated scavenging ratio was between 0.61 – 3.96 in the study area. It was obtained from the result that Au, Mn, and Zn were better removed by gravitational particle settling while Fe, Ti, and Rh were scavenged by precipitation. The results show extremely high levels of trace metals above prescribed thresholds, highlighting the need for international cooperation in resolving air quality concerns and developing regulations targeted at lowering emissions from the burning of solid waste in the study environment.

Forensic Elemental Analysis of Five Rupee and One Pound Coin with EDXRF Technique

Energy dispersive X-ray Fluorescence (EDXRF) technique using synchrotron radiation has been employed for elemental analysis of one pound and five rupees coins of two different countries- the UK and India. Total number of 12 coins - 4 one pound and 8 five rupees coin were analysed. A Peltier cooled Vortex solid state detector (SII Nano Technology, USA) having energy resolution of 138 eV at 5.96 keV X-rays was employed for the present analysis. A Peltier cooled Vortex solid state detector (SII Nano Technology, USA) having energy resolution of 138 eV at 5.96 keV X-rays was employed for the present analysis. The investigations were carried out to determine the similarities between the elemental composition and structure of coins. The major elements Cu, Ni, Fe, Cr and traces of two elements Mn and Mo were found during analysis. One of the elements i.e. Cu was found as primary major element in most of the coins. Two other elements Fe and Cr are also found as major element in 2 five rupees coins. Fe was generally considered as cheap metal composition in comparison to Cu. Besides these traces of Mo, S, Ca and Si were also observed whose compositional amount found very low (below 1%). The present study confirms the favorable economic conditions of two countries during their minting time. The XRF spectra and graphical representation of elemental concentration also helps to identify the similarities in structure and composition of coins. Results of present analysis of different types of coins are found in good agreement with standard composition and also with each other. The EDXRF analysis shows its effectiveness in forensic science without alteration of precious samples. Forensic analysis of such coins using Synchrotron radiation is very helpful in archeological study.

Performance evaluation of an online monitor based on X-ray fluorescence for detecting elemental concentrations in ambient particulate matter

Abstract. Knowledge of the chemical composition of particulate matter (PM) is essential for understanding its source distribution, identifying potential health impacts of toxic elements, and developing efficient air pollution abatement strategies. Traditional methods for analysing PM composition, such as collection on filter substrates and subsequent offline analysis with, for example, inductively coupled plasma mass spectrometry (ICP-MS), are time-consuming and prone to measurement errors due to multiple preparation steps. Emerging near-real-time techniques based on non-destructive energy dispersive X-ray fluorescence (EDXRF) offer advantages for continuous monitoring and source apportionment. This study characterizes the Horiba PX-375 EDXRF monitor by applying a straightforward performance evaluation including (a) limit of detection (LoD), (b) identification and quantification of uncertainty sources, and (c) investigation and comparison of measurement results from three contrasting sites in Luxembourg (urban, semi-urban, rural). We used multi-element reference materials (ME-RMs) from UC Davis for calibration and performed measurements during spring and summer 2023. The LoDs for toxic elements like Ni, Cu, Zn, and Pb were below 3 ng m−3 at 1 h time resolution. Higher LoDs were observed for lighter elements (e.g. Al, Si, S, K, Ca). Expanded uncertainties ranged between 5 % and 25 % for elemental concentrations above 20 ng m−3 and were maximal for concentrations below 10 ng m−3, reaching 60 %–85 %. Elemental analysis revealed S and mineral elements (Fe, Si, Ca, Al) as dominant contributors to PM10. Although the PM mass contribution of toxic trace elements (e.g. Zn, Cu, As) was generally very low, they were found to be enriched at the urban site Belvaux and the semi-urban site Remich compared to the more rural site Vianden. Our results explained on average 51 %–74 % of the gravimetric PM10 mass at the three sites. The study highlights the suitability and importance of the continuous PX-375 particle monitor for future air quality monitoring and source apportionment studies, particularly under changing emission scenarios and air pollution abatement strategies.

A provenance study on the ceramics excavated at the Varzaneh Plain, central Iran

Forty-six ceramic shards from the Early Bronze Age (EBA) archaeological site of Tappeh Gabri (the archaeological site 013), dated back to the latter half of the third millennium BCE and located at the Varzaneh Plain, central Iran, were studied using micro energy dispersive X-ray fluorescence (µ-EDXRF) and petrographic analysis. The precision and accuracy of quantitative data obtained by µ-EDXRF were tested using a series of geological certified reference materials (CRM). The expanded uncertainty and the Mantel test on data obtained by µ-EDXRF showed accurate and precise quantitative µ-EDXRF estimation of elements present in the CRMs above their quantification limit. We show that the majority of the ceramics at the Varzaneh Plain is most probably local product. Discussions prompted collecting further compositional data and performing petrographic investigation from the ceramic shards from southern and south-western Iran in order to shed light on the origin of the ceramic shards excavated at the Varzaneh Plain.

Effectiveness of energy dispersive X-ray fluorescence for the quantification of mineral elements in skim milk and whey powders

Milk and whey are subjected to quick deterioration due to bacterial growth. Turning them into powder allows for extended shelf life, easier storage, and more effective transport. Monitoring mineral elements in dairy powders is crucial for both technological and nutritional implications. Current analysis of minerals in food matrices is time consuming and requires high costs and labor. In this view, energy dispersive x-ray fluorescence (ED-XRF) may represent a potential alternative technique to rapidly determine mineral content of food matrices. The present study aimed to investigate the effectiveness of ED-XRF technique for the prediction of Na, Mg, P, S, K, Ca, Cu, and Zn in skim milk and whey powders. Reference analysis for mineral concentration in dairy powders was inductively coupled plasma optical emission spectrometry. The accuracy of ED-XRF for the prediction of mineral elements was assessed on all available samples (global calibration set; n = 23), and after splitting the whole data in a training set (n = 16) and a testing set (n = 7), comprising 70% and 30% of the available samples, respectively. The accuracy of prediction was moderate to low for Na and Mg, whereas robust predictions were obtained for P, S, K, Ca, Cu, and Zn, with coefficients of determination in global calibration from 0.88 to 0.99, and ratios performance to deviation in testing from 2.14 to 24.74. Results suggest that ED-XRF can be considered for accurate prediction of main mineral elements in dairy powders.

Functionally graded material for improved wear resistance manufactured by directed energy deposition

AbstractProtecting components against wear and corrosion is a common way to improve their lifetime. This can be achieved by coating them with a hardfacing material. Common coatings consist of materials such as tungsten carbide or cobalt-chromium alloys, also known as Stellite. Hardfacing materials can be deposited by welding methods like plasma welding or laser cladding. The discrete change of the base material to the hardfacing layer can lead to cracks and chipping. Studies showed a reduced risk of cracking when a functionally graded material is used to create a smooth transition between the base and the hardfacing. Gradings from austenitic steel to cobalt-chromium alloys are already known in the literature. However, there is no knowledge about austenitic- ferritic duplex steels as base material. Therefore, this study aims to demonstrate the feasibility of a functionally graded material from duplex steel to cobalt-chromium alloy with a new approach. By using powder-based directed energy deposition, a graded material with smooth material transition is manufactured additively. Cracking and porosity are examined through metallography. Microhardness measurements as well as the analysis of the chemical composition by energy dispersive X-ray spectroscopy and X-ray fluorescence are used to validate the build-up strategy.

Luminescence and scintillation characteristics of Ce3 + and Tb3+ co-doped SiO2 fiber for low-dose gamma radiation

Ce3+ and Tb3+ co-doped SiO2 optical fibers (SCTF) were prepared using the modified chemical vapor deposition method. The optical and structural properties of the SCTF samples were investigated using refractive index measurements, energy dispersive X-ray spectroscopy, photoluminescence (PL), transmission loss, and fluorescence lifetime. The SCTF was fabricated into a radiation dosimeter, and its gamma radioluminescence (RL) response was studied over a dose rate range of 424.27–2095.16 mGy/min and a total dose range of 424.27–2095.16 mGy. The radiation response exhibited good linearity. To verify the repeatability of the dosimeter, repeated experiments were conducted at a fixed dose rate of 2095.16 mGy/min. The results demonstrated that the dosimeter has good repeatability. An energy transfer model in SCTF was established, and Ce/Tb-doped SiO2 was prepared using a sol-gel method. The energy transfer model was verified by measuring its PL spectrum. The above results verify that the SCTF shifts the RL to a longer wavelength due to the energy transfer of radioluminescence, which is more conducive to the remote sensing and transmission of SiO2 optical fiber in an irradiated environment.

Hybrid-angle energy-dispersive X-ray diffraction and fluorescence system for the analysis of material in a vial

Hybrid-angle energy-dispersive X-ray diffraction and fluorescence system for the analysis of material in a vial

EDXRF and Machine Learning for Predicting Soil Fertility Attributes

Soil fertility evaluation is fundamental for sustainable agricultural practices, often relying on conventional laboratory methods. These methods, while accurate, are labor-intensive, time-consuming, and require chemical reagents. Spectroscopic sensors, such as energy-dispersive X-ray fluorescence (EDXRF), offer a rapid and non-destructive alternative but require calibration of machine learning models for accurate prediction of fertility attributes. In this context, this study compares the performance of four machine learning algorithms—multiple linear regression (MLR), partial least square regression (PLS), support vector machine regression (SVM), and random forest regression (RF)—in predicting soil pH, organic carbon (SOC), sum of exchangeable bases (BS), and cation exchange capacity (CEC) using EDXRF data from two soil datasets. Results indicate that PLS models outperformed others (the hierarchy of accuracy was PLS > MLR > SVM > RF). Overall, we emphasize the benefits of integrating PLS with EDXRF, capable of mitigating the use of traditional soil analysis.

Determination of trace heavy metal ion Tl(I) in water by energy dispersive X-ray fluorescence spectrometry using prussian blue dispersed on solid sepiolite

X-ray fluorescence (XRF) offers the advantage of performing measurements without damaging or consuming the sample, enabling rapid and simultaneous multi-element analysis. It has been widely applied in environmental monitoring, materials science, geology, and medicine, but not in water. Here, a novel method is proposed that combines energy-dispersive X-ray fluorescence spectroscopy (EDXRF) with prussian blue dispersed on solid sepiolite nanomaterials (PB/SEP) and an integrated enrichment-separation device to detect trace heavy metal ion Tl(I) in water environments. The water sample passes through the detachable enrichment component, and subsequently, PB/SEP is used as a solid adsorbent for the pre-enrichment of Tl(I) in the water sample. This process eliminates the cumbersome separation steps and saves analysis time. The research elucidates the impact of sample pH, flow rate, volume, and interfering ions on elemental recoveries, demonstrating that the proposed method offers a low detection limit of 0.057 μg/L, but also maintains high precision, with the RSD of less than 4.39 %. Furthermore, the PB/SEP magnetic nanocomposite was successfully applied to the tap water sample and river water sample with recoveries ranging from 93.5 % to 128.3 %, confirming the accuracy and practicality of the analytical method.