Energy Dispersive X-ray Fluorescence Spectrometry Research Articles

Studies on the Authorship of Albumen Vintage Photographs: A Combined Experimental and Chemometric Approach

The differences in albumen photographs from vintage photographic studios were identified by energy-dispersive X-ray fluorescence spectroscopy and Fourier transform infrared spectroscopy. The results inspired the concept of finding common features characteristic of a given photographic studio. The obtained measurement data (i.e., positions of vibrational bands for characteristic groups of albumen and the mass contents of chosen elements) were analyzed chemometrically by employing the Principal Component Analysis (PCA). The PCA technique allowed us to reduce the number of relevant experimental parameters characterizing the unique features of the photographic objects. The two major components were able to distinguish the photographic objects in terms of their authorship and the time to produce a photograph. The method developed was examined for a selected group of photographs consisting of albumen prints from three Polish photographic ateliers. To validate ED-XRF measurements and, consequently, the chemometric findings, reference albumen photo samples were designed and prepared. The empirical functional relationships between the content of photochemically reduced silver particles on the photographic paper and several physicochemical factors, including time of exposure to UV light, AgNO3 concentration in a fixed bath, and concentrations of other additives, were proposed. These results can be used for the prediction of the experimental conditions under which the investigated photographs were developed.

Fast, accessible and reliable method for elemental analysis of metals in solution by ED-XRF spectroscopy

The measurement of metals in solution is usually performed using inductive coupled plasma hyphenated techniques or atomic absorption. Although very sensitive and accurate, these analytical techniques are quite expensive and do not allow field measurements. The present work takes advantage of energy-dispersive X-ray fluorescence (ED-XRF) ease-of-use features to determine the concentration of rare earth elements (Y, Pr, Nd, Eu) and others (S, Fe, Ni, Cu, Zn) in aqueous solutions, after appropriate sample treatment. The approach turned out to be a reliable and very convenient procedure for field analysis. The simplicity, speed and reliability of the methodology used combined with the possibility of simultaneous analysis and low cost of the method can be advantageous in industrial context. The approach relies on the suspension of the target solutions in a cellulose matrix that is further converted into a pellet for direct analysis. Calibration curves obtained by regression analysis at 5% significance are shown for a variety of elements (S, Fe, Ni, Cu, Zn, Y, Pr, Nd, Eu) with correlation coefficients between 0.9555 and 0.9980. Higher coefficients of variance were obtained for the calibration of S and Pr due to low sensitivity and the overlapping with the L lines of Nd, respectively. The performed calibrations were not affected by the presence of other analytes in the matrix. Results obtained showed that it is possible to use the proposed methodology to accurately quantify d and f block metals in aqueous solutions by ED-XRF after sequestering the chemical content into a cellulose powder matrix and further processing into a pellet.Graphical

Application of handheld/portable spectroscopic tools to the identification, inner stratigraphy and mapping of archaeological metal artefacts

Abstract Field handheld/portable instrumentations, such as in-situ geochemical analyzers, have the potential to assist efficiently targeted geochemical archaeometry campaigns in detecting and quantifying specific elements. Non-destructive portable Energy Dispersive X-Ray Fluorescence (ED-XRF) and micro-destructive handheld Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation were utilized to investigate the elemental composition, internal stratigraphy by depth profiling and microscale compositional mapping of five copper and two iron alloy artefacts collected from various ancient graves in the Minervino Murge area, Apulia, Italy. The primary elements identified by both techniques included Cu, Sn and Pb in copper alloys, and Fe with minor amounts of Cu and Pb in iron alloys. Furthermore, the elements Al, Ca, Si, Mg, Na and K, mostly originated from soil contamination, and the trace elements Sb, Ni and Zn were detected. The satisfactory performance of both techniques was assessed by their capacity to provide reproducible elemental composition data. Finally, the depth profile and mapping achieved by LIBS contributed to understanding the metal processing and history of the objects studied, so confirming both techniques to be robust analytical tools in outdoor archaeology and archaeometry campaigns.

ZnS@ fluorenone derived multifunctional quantum dots for simultaneous recognition of bovine serum albumin (BSA) and copper ions (Cu2+) in aqueous blood and urine samples

An efficient synthesis of water-stable and fluorescent ZnS quantum dots has been executed beginning with its organic predecessor possessing fluorenone for sensing bovine serum albumin (BSA) among other proteins. Moreover, the organic predecessor of quantum dots has also been utilized for sensing of F- ions with binding constant of 1.8 × 104 M−1. Various spectroscopic techniques such as high-resolution transmission electron microscopy (HRTEM), powder X-ray diffraction (PXRD), UV-visible (UV-vis), Fourier transform infrared (FTIR), thermogravimetric (TGA), Energy dispersive X-ray analysis (EDX), circular dichroism (CD) and Fluorescence (FL) spectroscopy have been utilized for the characterization of the developed quantum dots. The emission properties of quantum dots made them useful for the sensing of BSA and Cu2+ accompanied with secondary sensing of urea. The LODs value for BSA and Cu2+ were calculated as 213 and 211 nM, respectively. Demonstrating remarkable efficacy, these quantum dots have been successfully employed for the discernment of BSA in human blood and urine samples, achieving an outstanding recovery rate of up to 99.8%.

Influence of fluoride characteristics on tooth surface protection in an erosive condition: A multifaceted characterization approach.

To evaluate the effect of fluoride consistency and composition to protect enamel and dentin against the dental erosion. Bovine enamel and dentin specimens were treated with artificial saliva, neutral fluoride gel (NFG), acidulated phosphate fluoride gel (AFG), neutral fluoride foam (NFF), and acidulated phosphate fluoride foam. The samples were subjected to cycling. Micro energy-dispersive X-ray fluorescence spectrometry, surface roughness (Ra), contact angle (CA), and scanning electron microscopy (SEM) were performed. Composition, CA and Ra data were analyzed by ANOVA and multiple comparison test (p < 0.05). The dentin protected had a significantly higher mineral content than in the control. Eroded unprotected enamel had higher Ra values than normal surfaces. Fluoride treatments increased the Ra in dentin samples. AFG increased the CA in enamel. Fluoride foams increased CA in dentin with reduced mineral loss. SEM analysis found a deposited layer on enamel treated with AFG and remnants of deposits on dentin treated with NFG and NFF. Regardless of the form of application, fluoride provided protection against erosion, however with different levels. Applying the adequate fluoride form is relevant since the formulations have different effects on both enamel and dentin.

Combined use of principal component analysis/multiple linear regression analysis and artificial neural network to assess the impact of meteorological parameters on fluctuation of selected PM2.5-bound elements.

Based on the data of the State of Global Air (2020), air quality deterioration in Thailand has caused ~32,000 premature deaths, while the World Health Organization evaluated that air pollutants can decrease the life expectancy in the country by two years. PM2.5 was collected at three air quality observatory sites in Chiang-Mai, Bangkok, and Phuket, Thailand, from July 2020 to June 2021. The concentrations of 25 elements (Na, Mg, Al, Si, S, Cl, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Br, Sr, Ba, and Pb) were quantitatively characterised using energy-dispersive X-ray fluorescence spectrometry. Potential adverse health impacts of some element exposures from inhaling PM2.5 were estimated by employing the hazard quotient and excess lifetime cancer risk. Higher cancer risks were detected in PM2.5 samples collected at the sampling site in Bangkok, indicating that vehicle exhaust adversely impacts human health. Principal component analysis suggests that traffic emissions, crustal inputs coupled with maritime aerosols, and construction dust were the three main potential sources of PM2.5. Artificial neural networks underlined agricultural waste burning and relative humidity as two major factors controlling the air quality of Thailand.

Biopolymeric fibers prepared by centrifugal spinning blended with ZnO nanoparticles for the treatment of Acne vulgaris

Acne vulgaris is a serious dermatological disease affecting a significant part of the population. Currently, available therapeutics are effective only at high concentrations, which has a negative environmental and economic impact. In particular, ZnO nanoparticles (NPs) have a great potential in various biomedical applications due to their specific properties and antibacterial/antiviral activity. In this study, biomedically approved ZnO NPs with distinct diameter were used as the active therapeutic modality to treat acne-causing pathogens. For the first time, we show the utilization of ZnO NPs that were evenly distributed within centrifugally spun fiber carriers. Upon application on the skin, ZnO NPs can sustainably release and have profound antibacterial activity at lower therapeutic concentrations. Fibers were made using innovative centrifugal spinning procedure from natural polymers - gum arabic and pullulan - that are known for their biocompatibility. Different amount of ZnO NPs (from 0.03 to 4.5 wt.% related to the dry mass) was added into the spinning polymer solution, either in a form of a dry powder or as a dispersion containing NPs and isopropyl myristate. The resulting fibers were subsequently characterized for morphology and presence of ZnO NPs by Scanning Electron Microscopy and Energy-Dispersive X-ray fluorescence spectrometry. The materials were thoroughly assessed for their antibacterial activity against Cutibacterium acnes and Staphylococcus epidermidis, which are major opportunistic pathogens causing acne. The combination of two types of nanomaterials, namely active nanoparticles and fiber carriers, proved to be very promising and bear a great potential for the treatment of these diseases.

Evaluation of ED-XRF for the detection of inorganic adulterants in turmeric, paprika and oregano

Herbs and spices are known to be prone to food fraud and accurate analytical tools are needed to detect adulterants. Amongst the potential adulteration, dilution with bulking agents has regularly been reported, especially with inorganic materials such as talc or brick powder. Energy Dispersive X-Ray Fluorescence (ED-XRF) spectrometry is a well-established non-destructive analytical technique for qualitative and quantitative elemental analysis of a wide variety of samples. ED-XRF was here evaluated for the detection of inorganic adulterants in turmeric, paprika and oregano, which were selected as representative for the herbs & spices food category. Magnesium, silicon, and calcium were identified as elements to detect talc, soapstone, brick/clay powder, and chalk inorganic adulterants. ED-XRF successfully detected adulterated samples when spiked down to 5% (w/w) in the selected herbs and spices. With its ease-of-use and speed, ED-XRF is well adapted for the monitoring of inorganic adulteration of herbs and spices along the supply chain.

Critical evaluation of energy dispersive X-ray fluorescence spectrometry for multielemental analysis of coffee samples: Sample preparation, quantification and chemometric approaches

In the present contribution, a critical evaluation of the use of EDXRF (Energy dispersive X-ray fluorescence spectrometry) for elemental composition determination (K, Ca, Mn, Fe, Cu, Zn, Sr and Rb) of coffee samples is presented. Firstly, several sample treatment procedures (pressed pellets and loose powder) and quantification strategies (fundamental parameters and empirical calibration) were evaluated.In addition to quality and nutritional purposes, information of elemental content in coffee samples can be also useful for coffee traceability and provenance studies. In view of that, a comparison of different tools such as explorative principal component analysis (PCA) and classification by partial least square regression (PLS-DA) were also tested as discriminating tools of different types of coffee samples (i.e., pure, instant and coffee with additives). Chemometric analysis was performed using coffee elemental concentrations determined by the developed EDXRF method and, for the first time, using raw EDXRF spectra obtained, without the need of a fitting and quantification procedure.

Common myrtle (Myrtus communis L.): Trace element composition and contribution to dietary intake

Common myrtle (Myrtus communis L.) is an appreciated aromatic and medicinal plant used as a flavor and fragrance ingredient in culinary applications, and possesses several bioactive compounds with marked health benefits. In the present investigation selected mineral and trace element concentrations were measured in Algerian myrtle leaves by energy dispersive X-ray fluorescence (EDXRF) spectrometry. The results show that K, Fe and P were present in high amounts with mean values of 17,971 ± 17.9, 750 ± 17 and 705 ± 11 μg–1 respectively. The decreasing sequence of the mean contents of essential elements in M. communis is as follows: K > Fe > P > Mn > Zn > Cu > V > Cr. The estimation of daily intake through the consumption of 10 g DW day−1person−1 contributes sufficiently or partially to the daily needs of some essential elements such as Fe, V, Cr, and Mn. Toxic element concentrations (As and Br) were found inferior than the set limits according to the world health organization (FAO/WHO). These results provide a new data reference for pharmaceutical and culinary purposes.

Synthesis of NaA Zeolite: Conventional Route and Green Route

The research describes a sustainable approach for the synthesis of zeolite NaA using kaolin as an alternative source of silica. The main objective of this research was to prepare NaA zeolite using metakaolin derived from kaolin from the state of Rio Grande do Norte, Brazil, as an alternative source of silica, reducing the production cost and evaluating its thermal stability. In addition, a study of the thermal stability of the zeolite and cost estimates for zeolite production were carried out. Traditional methods of zeolite synthesis, mainly through hydrothermal processes, are often associated with high costs, waste generation, and negative environmental impacts. This work addresses these concerns by exploring a more sustainable approach. The kaolin used in the study was characterized by X-ray diffraction, energy-dispersive X-ray fluorescence spectroscopy, infrared spectroscopy, and thermogravimetry. These techniques help confirm the composition and properties of the raw material. NaA zeolite was synthesized by replacing sodium silicate with metakaolin using the hydrothermal synthesis method. The NaA zeolite was characterized by XRD and IR, which helped verify its purity and structural order. The study's results demonstrated that kaolin waste mainly consists of kaolinite, which suggests that it can be effectively used as a source of silica. Furthermore, the research successfully produced low-cost NaA zeolite in a relatively short synthesis time, achieving high purity and structural order. The study highlights the potential of using kaolin waste as a sustainable source of silica for zeolite production, helping to minimize environmental impacts and reduce processing costs compared to traditional methods. This work presents a promising and sustainable method for producing NaA zeolite from kaolin waste, which has the potential to contribute to cost reduction, waste reduction, and improved environmental sustainability in zeolite production processes. This research is aligned with the broader goals of reducing the ecological footprint of industrial processes while maintaining product quality and efficiency.

DETERMINAÇÃO MULTIELEMENTAR EM AMOSTRAS DE BIODIESEL EMPREGANDO ESPECTROMETRIA DE FLUORESCÊNCIA DE RAIOS-X POR DISPERSÃO DE ENERGIA APÓS EXTRAÇÃO INDUZIDA POR QUEBRA DE EMULSÃO

MULTI-ELEMENT DETERMINATION IN BIODIESEL SAMPLES USING ENERGY DISPERSIVE X-RAY FLUORESCENCE SPECTROMETRY AFTER EXTRACTION INDUCED BY EMULSION BREAKING. A method for determining Cd, Cr, Cu, and Fe in biodiesel samples is proposed using energy dispersive X-ray fluorescence spectrometry (EDXRF) after extraction induced by emulsion breaking (EIEB). A volume of 7.0 mL of biodiesel and an aliquot of 500 µL of Triton X-100 solution (2%, v v-1) prepared in nitric acid were used to prepare the emulsion. After 5 min of manual agitation, phase separation was performed by centrifugation for 5 min at 2000 rpm. A 100 µL aliquot of the enriched aqueous phase was collected and applied to the center of a filter paper. After drying, the analysis was performed directly on the paper using EDXRF. The detection limits were 60, 20, 30, and 60 μg kg-1 for Cd, Cr, Cu, and Fe, respectively. Recovery tests were performed by adding 450 μg kg-1 of the analytes in biodiesel samples, and the results varied between 87 and 113%. The procedure was applied to biodiesel samples, and the concentrations obtained for the four analytes were compared with those obtained by inductively coupled plasma optical emission spectrometry (ICP OES) after sample digestion.

SURFACE PATINA AND CLAY CHARACTERIZATION: MULTI-ANALYTICAL INVESTIGATIONS INTO BIDRI HANDICRAFT

Bidri handicraft in India, patronised by Bahamani kings, dates back to the fifteenth century and is nowadays under operational and socio-economic threats. The craft is made of zinc alloy, which poses scientific challenges in the areas of metallurgy, metal oxidation, and surface science. In the present paper, the art, owing to its scientific enigma, is under scrutiny, wherein the handicraft mandates the use of Bidar Fort (in Karnataka, India) clay, which bestows the handicraft its characteristic matt-black patina. The fort is a heritage conservation site and thus poses a threat to the perennial practice of handicraft. Therefore, it is imperative to document the patina and fort clay. Thus, morphological and chemical characterization of Bidri artefact surfaces was accomplished using scanning electron microscopy (SEM), X-ray Diffraction (XRD) analysis, X-ray Photoelectron Spectroscopy (XPS), and Energy Dispersive X-ray fluorescence spectroscopy (ED-XRF); besides, elemental characterization of Bidar fort clay was accomplished using SEM coupled with energy dispersive X-ray spectroscopy (EDS). This study is significant, as it is one of the initial works to scientifically document Bidri handicraft surface and clay, besides laying the foundation for future studies; a step to conserve the handicraft; and a step to prevent the deterioration of the Bidar fort monument.

Fabrication and characterization of thin 94Zr target with gold backing for nuclear lifetime measurements using DSAM

For lifetime measurements of excited nuclear states in the sub-picosecond range, a thin target with a thick backing of high-Z material is required. To meet these specifications, a thin isotopic94Zr target of thickness 1.14 ± 0.05 mg/cm2, with backing of 4.7 ± 0.2 mg/cm2 thick Au layer, has been fabricated using the cost-effective cold rolling technique at the target laboratory of Inter-University Accelerator Centre (IUAC), New Delhi. The thickness verification and purity check of the fabricated target have been carried out by non-destructive Energy Dispersive X-ray Fluorescence (EDXRF) and Rutherford Backscattering Spectrometry (RBS) techniques. The results of these measurements are in good agreement with each other. The elemental composition, purity and surface morphology have been explored by Energy Dispersive X-ray Spectrometry (EDS) and Scanning Electron Microscopy (SEM) techniques. The fabricated target has been successfully used with a16O ion beam in a recent γ-ray spectroscopy experiment for lifetime measurements using the Doppler Shift Attenuation Method (DSAM) at IUAC, New Delhi.

Quantitative analysis of energy-dispersive X-ray fluorescence spectroscopy based on machine learning and a generative data enhancement technique

This paper proposes a data enhancement technique to generate expanded datasets for machine learning by developing an X-ray fluorescence spectra simulator based on the physical process. The simulator consists of several modules, including the excitation source, the interaction process, and the detection system. The spectra generated by the simulator are subject to dimension reduction through feature selection and feature extraction algorithms, and then serve as the input for the XGBoost (extreme gradient boosting) model. Six elements of metal samples with various content ranges were selected as the research target. The results showed that for simulated data, the R2 value for elements with concentrations ranging from 0% to 100% is greater than 95%, and for elements with concentrations of &lt;0.3%, the R2 value is greater than 85%. The experimental data were predicted by the model trained by the simulated spectra. Therefore, this approach provides reliable results for practical application and can supply additional datasets to obtain reasonable prediction results for machine learning with inadequate reference materials.

Characterization of a Unique Nuragic Bronze Navicella with a Combination of X-ray Fluorescence Spectrometry and Monte Carlo Simulation

This paper describes the results obtained from an archaeometric study of a bronze Nuragic small boat model (Sardinia, Italy) dating from the Early Iron Age (presumably 9th–7th centuries BC). The artifact comes from an unknown location in Sardinia and is one of the objects that came to the Museum of Turin in the 19th century. This model is of particular interest as it is a unique Nuragic boat model containing a human figure among its decorations. The artifact is kept in the collection of the Royal Museum of Turin (Italy) and is a typical example of Sardinian manufacture from the Early Iron Age. This study was carried out using a combination of non-invasive techniques with energy dispersive X-ray fluorescence spectrometry (ED-XRF) integrated with Monte Carlo (MC) simulations and Raman spectroscopy, which allowed the characterization of the alloy of the artifact.

Analysis of Heavy Metals and Other Elements in Soil Samples for its Physicochemical Parameters Using Energy Dispersive X-Ray Fluorescence (EDXRF) Techniques

The present study was conducted to determine the physicochemical properties and the composition of trace elements of soil samples in agriculture lands. This study has been designed to analyze heavy metal contaminations in 12 soil samples collected at a depth 0-20 cm from the agriculture areas of Munshiganj using Energy Dispersive X-Ray Fluorescence (EDXRF) spectroscopy. This study revealed that the maximum Ca, Ti, Mn, Fe, Cu, Zn, Rb, Sr, and Pb contents in soil samples were 76293, 3911, 534, 44652, 57.50, 532, 101.45, 242.11 and 39.31 mg/ kg respectively. A physicochemical study of soil is based on various parameters like soil PH, electrical conductivity (EC), TDS mg/L, Salinity. The value of soil PH found to be 7.53 to 9.24, conductivity was ranging from 22.4-66.5 μs, Total Dissolved Solid (TDS) was ranging from 13.39-37.70mg/L and salinity was ranging 22.40-66.50 μs. Along with the experimental data, several environmental indices (Contamination factor, geo-accumulation index, enrichment factor, pollution load index, Quantification of Anthropogenic Concentration of Metal (QoC) have been identified for comprehensive assessment of our study site, which suggesting that these heavy metals Ca, Ti, Mn, Fe, Cu, Zn, Rb, Sr, and Pb might come in the samples due to anthropogenic activities.

Fingerprint of Precious Metals Ornaments to Post-Mortem Inventory by Energy Dispersive X-Ray Fluorescence Spectrometry

Fingerprint of Precious Metals Ornaments to Post-Mortem Inventory by Energy Dispersive X-Ray Fluorescence Spectrometry

The composition of roman metals from Moinho do Castelinho and Quinta da Bolacha (Portugal)

The work involved the elemental characterisation by micro energy-dispersive X-ray fluorescence spectrometry of copper-based objects recovered during archaeological works at the neighbouring roman sites of Moinho do Castelinho and Quinta da Bolacha (Lusitania province). The set of 9 artefacts comprised ornaments, tools and implements of different type (fibula, shroud pin, punches, spatula, hook and nail), in addition to small fragments of unknown functionality (a fragmented handle and a small bar). Micro-EDXRF point analyses identified a diversified metallurgy including copper, bronze and leaded bronze, in addition to iron, nickel, arsenic and antimony as minor elements. Furthermore, micro-EDXRF elemental mappings identified the presence of Pb-rich inclusions in the bronze alloys with higher lead content. The composition of these roman artefacts suggests a selection of alloys according to the functionality of the artefact, as evidenced by a nail composed of copper, a handle with a more complex shape made with leaded bronze and a bronze fibula with a higher amount of tin. Finally, the choice of distinct alloys for everyday objects was viewed in the light of technological, symbolic and economic concerns, and compared with the use pattern of roman sites in the western end of the Iberian Peninsula.

Physicochemical characterization of Copper Ore from Akiri, Awe LGA, Nasarawa State

The bulk density, compressional strength, hardness, particle study and chemical analysis of ore from Akiri were determined using standard methods and Energy Dispersive x-ray Fluorescence spectrometry (ED-XRFS). The results obtained indicated that the ore bulk  density was 3.58 (g/cm3 ), compressional strength 1.24 (%), and hardness 96.0(N). The particle size analysis of +0-90µm, +125-90µm, and  +125-180µm, revealed over-size fractions above 250µm.The chemical composition of the ore in terms of oxide showed that the ore is  composed of different minerals: 63.52% Fe2O3, 11.25% SO3, 7.62% CuO, 4.30% MOO3, 3.18% SiO2, 1.73% BaO,1.20% ZnO,1.12%  MnO,0.86% PbO,0.60% Re2O7, 0.54% Eu2O3and CaO, 0.27% RuO2, 0.15% Cr2O3, 0.09% K2O, 0.08% Yb2 O3, 0.06% SrO, and TiO2, 0.04%  Nd2O3, and CeO2, 0.03% Y2O3 and NiO respectively. The results of the elemental composition varied in the copper ore with an indication  of a significant concentration of Cu compared to other elements, except Fe which showed a higher concentration. The value 35.% Fe,  6.10% Cu, 4.48% S, 3% Mo, 1.55% Ba, 1.48% Si, 1% Zn and Pb, 0.90% Mn, 0.5% Re, 0.45 Eu, 0.40% Ca, 0.21% Ru, 0.10% Cr, K, and Yb,0.04% Ti,  Ni, Y, and Sr, 0.03 % Nd, and Ce obtained represent the individual elemental content in the ore. The result is an indication that the ore can  be explored for the processing of valuable minerals.