Energy Dispersive X-ray Fluorescence Research Articles

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%.

XRF calibration with low-cost samples and implementation for quantification of inorganic elements in lipsticks

In this paper, the preparation of low-cost samples, for the calibration of an energy–dispersive X-ray fluorescence system is presented. The entire procedure is proposed as an undergraduate or postgraduate student laboratory activity, which aims to familiarize students with the procedure of calibration of a spectroscopy-based analytical method through the XRF technique. Furthermore, the use of XRF for the determination of elemental concentrations in samples related to students’ interests, was attempted.

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.

Maximization of the blue-white contrast of ancient porcelain decorations from Jingdezhen imperial kiln by Co-spinel formation

By analyzing the chromaticity values of the ancient blue-and-white porcelain combined with the imitated experiment, the color information is quantified and ‘color dispersion’ mechanism is clarified. Energy Dispersive X-Ray Fluorescence (EDXRF), field emission scanning electron microscopy (FE-SEM), the advanced focused ion beam transmission electron microscopy (FIB-TEM) technique, etc, were used to study the characteristics and the ‘color dispersion’ mechanism of the blue-and-white porcelain in Jingdezhen imperial kiln. The ‘color dispersion’ of the blue-and-white porcelain is mainly caused by Co-element structure stability, which is verified by the archaeological experiment results. Blue-and-white decoration lines diffusion length (named as ‘color dispersion’) are long (i.e. fuzzy) which has few or no spinel crystals in the body-glaze interaction layer of the blue-and-white porcelain. However, the blue and white porcelain with the clear lines has a large number of spinel crystals. The experimental results enrich the literature on the history of ceramic manufacturing techniques in Jingdezhen.

Environmentally friendly binders from calcium carbide residue and silica fume and feasibility for soft clay stabilization

This investigation elucidates the development of an innovative, sustainable binder derived from calcium carbide residue and silica fume, aimed at enhancing soft clay stabilization with minimal environmental impact. Various mixtures were examined, focusing on the CaO to SiO2 molar ratio (Ca/Si), which varied from 1.85 to 0.65. Comprehensive analyses of the raw materials and pastes, including chemical composition, phase evolution, and microstructure, were conducted using techniques like Energy dispersive X-ray fluorescence, X-ray diffraction, thermogravimetric analysis, and scanning electron microscopy. Results indicate a significant impact of raw material fractions on the compressive strength and cementitious properties. The mixture with a Ca/Si of 1.55 demonstrated the highest long-term strength, attributed to increased C–S–H content. A mixture of 30 wt% calcium carbide residue and silica fume was found to improve the unconfined compressive strength of soft Bangkok clay by 84% compared to 10 wt% ordinary Portland cement, demonstrating its efficacy and potential for widespread application in green construction initiatives. This research not only promotes the recycling of industrial by-products, reducing environmental impact, but also represents a significant advancement in sustainable construction materials.

Fabrication and characterization of new Fe3O4@SiO2@TiO2-CPTS-HBAP (FST-CH) nanoparticles for photocatalytic degradation and adsorption removal of rhodamine B dye in the aquatic environment

In this study, Fe3O4@SiO2@TiO2-CPTS-HBAP (FST-CH) nanoparticle was prepared for the simultaneous adsorption and photocatalytic degradation of aromatic chemical pollutants (Rhodamine B dye) in aqueous solution. FST-CH nanoparticle was characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), Energy Dispersive X-Ray (EDX) Fluorescence Spectrometer and X-Ray Diffraction (XRD) spectroscopy. The photocatalytic activity of rhodamine B dye (RhB) was evaluated with a Kerman UV 8/18 vertical roller photoreactor. About 56% of RhB in aqueous medium was adsorbed by FST-CH nanoparticles with only 45 min of stirring in the dark, and about 77.01% was degraded or converted to other structures under the photoreactor for 120 min. The photocatalytic degradation of RhB (apparent rate constant: 0.0026 mg dm−3 min−1) occurred by a pseudo-second order reaction. In addition, the recovery of the prepared magnetic FST-CH nanoparticle by an external magnetic field, exhibiting good magnetic response and reusability, shows that the obtained magnetic FST-CH nanoparticle is stable and maintains high degradation ratio and catalyst recovery even after four cycles. Thus, the prepared FST-CH nanoparticle can be highly recommended for its use in potential applications of water decontamination.

Analysis the Metal Composition of Fish Samples Collected From Karacaören II Dam Lake

The objective of this study was to analyze the metal content in the organs of Oncorhynchus mykiss, commonly known as rainbow trout, at 12 different locations within the cages located in Karacaören II Dam Lake. The metal contents in fish samples were analyzed using a PANalytical Epsilon5 energy dispersive X-ray fluorescence (EDXRF) spectrometer. We will analyze the findings by displaying the fluctuating metal concentrations in various internal organs over the seasons.

Possibilities of various arrangements of X-ray fluorescence analysis in the study of paintings

Energy dispersive X-ray fluorescence analysis (EDXRF) is a very useful method of elemental analysis in the study of works of art and archaeological finds, allowing the simultaneous non-destructive identification of a number of elements. A certain problem, if samples are not to be extracted from the investigated artifact, is its small depth range. However, this is not a serious drawback when it comes to the analysis of thin layers, such as plating or painting.In our laboratory, XRF was gradually developed and the equipment improved, with one of the main goals being the study of archaeological finds and works of art for the purposes of learning about the cultural heritage and restoration works.The presented paper aims to compare the possibilities of different macro- and micro-XRF instrumental arrangements in the study of paintings, from fast orientational measurement with a compact hand-held device through 2D scanning with a collimated beam to 3D analysis with collimated X-ray optics. Attention is paid to both the advantages and limitations of individual arrangements. A small painting by A. Piepenhagen, a typical representative of 19th century romantic landscape painting, was chosen as the object on which the possibilities of individual XRF variants are demonstrated.

X-ray fluorescence analysis in the study of paintings – an overview

Energy dispersive X-ray fluorescence analysis (EDXRF) is an excellent method in investigations of cultural heritage treasures, including easel and wall paintings and illuminations in ancient manuscripts. As one of the few methods applicable for this purpose, it is non-destructive and non-invasive. It is often combined with other methods such as optical microscopy, visible light photography, UV fluorescence photography, infrared reflectography, Fourier transform infrared spectroscopy, X-ray radiography, Raman spectrometry and others. The complex layered structure and mixtures of pigments, especially on easel paintings, represent a challenging task from the point of view of analysis. However, without taking samples it is only possible to analyse the thin surface layer of the investigated object with a thickness of tens to a few hundreds of micrometres. Nevertheless, this is not too much a problem when analysing paintings and even more so in the analysis of illuminations in manuscripts. The paper has an overview character and aims to summarise the possibilities, advantages and problems of XRF in this area and to demonstrate them on selected examples of published works, which in some cases are devoted to the works of leading painters from various historical periods (Giotto di Bondone, Antonello da Messina, Raffaelo Sanzio, Antonio Allegri da Corregio, Anthonis van Dyck, Rembrandt van Rijn, Giorgio Marini, Pablo Picasso and others). This review includes also a brief mention of selected research carried out in our laboratory.

Quantitative analysis of iodine and bromine in soil using an energy-dispersive X-ray fluorescence spectrometer with three-dimensional polarized optics.

A nondestructive and simple method for the determination of bromine and iodine in soil was investigated using an energy-dispersive X-ray fluorescence spectrometer equipped with three-dimensional polarized optics. Using a gadolinium X-ray tube and Mo and Al2O3 as optimal secondary target materials, K-lines were detected for bromine and iodine. The minimum detection limits for bromine and iodine were calculated using JSAC0411, a certified reference material of soil for metal composition analysis, and were 0.77mg/kg for bromine and 2.3mg/kg for iodine at a measurement time of 600s. The results of the determination of bromine and iodine in soil samples by the standard addition method were 256 ± 8mg/kg for iodine and 67.9 ± 1.3mg/kg for bromine with JSAC0411, which were in close agreement with the results measured by inductively coupled plasma mass spectrometry (ICP-MS) after alkaline extraction with tetramethylammonium hydroxide (TMAH) solution. The method developed in this study is an excellent technique for direct analysis of soil by X-ray fluorescence analysis without any pretreatment such as alkaline extraction. It is expected to be a practical analytical method for elucidating the dynamics of bromine and iodine in agricultural land and soil.

Electronic waste analysis using laser-induced breakdown spectroscopy (LIBS) and X-ray fluorescence (XRF): Critical evaluation of data fusion for the determination of Al, Cu and Fe

BackgroundElectronic waste (e-waste) proliferation and its implications underscore the imperative for advanced analytical methods to mitigate its environmental impact. It is estimated that e-waste production stands at a staggering 20–50 million tons yearly, of which merely 20–25% undergo formal recycling. The e-waste samples evaluated contain computers, laptops, smartphones, and tablets. ResultsForty-one samples were processed, involving the disassembly and separation of components. Subsequently, two analytical techniques, laser-induced breakdown spectroscopy (LIBS) and energy dispersive X-ray fluorescence (ED-XRF), were applied to quantify aluminum (Al), copper (Cu), and iron (Fe) in the e-waste samples. The samples were then analyzed after acid mineralization with 50% v v−1 aqua regia in a digester block and finally by ICP OES. A solid residue composed of Si and Ti was observed after the digestion of the samples. Multivariate calibration strategies such as partial least-squares regression (PLS), principal component regression (PCR), maximum likelihood principal component regression (MLPCR), and error covariance penalized regression (ECPR) were used for calibration. Finally, the figures of merit were calculated to verify the most suitable models. The results revealed robust models with notable sensitivity, varying from 8.98 to 35.04 Signal (a.u.)(% w w−1) −1, low Limits of Detection (LoD) within the range of 0.001–0.2 % w w−1, and remarkable relative errors ranging from 2% to 33%, particularly for Cu and Fe. SignificanceNotably, the models for Al faced inherent challenges, thus highlighting the complexities associated with its quantification in e-waste samples. In conclusion, this research represents an important step toward a more sustainable and efficient future for electronic waste recycling, signifying its relevance to global environmental welfare and resource conservation.

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.

Adsorption of Methylene Blue Dye and Analysis of Two Clays: A Study of Kinetics, Thermodynamics, and Modeling with DFT, MD, and MC Simulations.

The purpose of this research was to learn more about the primary and secondary properties of Moroccan natural clay in an effort to better investigate innovative adsorbents and gain access to an ideal adsorption system. Scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy analysis (SEM-EDX) and X-ray fluorescence were employed for identification. SEM revealed clay grains, including tiny particles and unevenly shaped sticks. First- and second-order rate laws, representing two distinct kinetic models, were applied in the kinetic approach. Adsorption of dye MB onto natural clay was studied, and the results agreed with the 2 s order model. The significant correlation coefficients support the inference that the adsorption process was governed by the Langmuir model. Subsequent DFT analyses demonstrated that the methylene blue dye's HOMO and LUMO surfaces are dispersed across most of the dye's components, pointing to a strong interaction with the clay. To determine how the dye might be adsorbed onto the clay, we employed quantum descriptors to locate its most nucleophilic and electrophilic centers. Endothermic reactions are evident during the MB adsorption process on clay, as indicated by the positive values of ΔH0 and ΔS0 (70.49 kJ mol-1of RC and 84.19 kJ mol-1 of OC and 10.45 J mol-1 K-1 of RC and 12.68 mol-1 K-1 of OC, respectively). Additionally dye molecules on the adsorbent exhibit a higher order of distribution than in the solution, indicating that the adsorption process is spontaneous.

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.

An Experimental Examination on the Determination of γ-ray Shielding Parameters of Some Dielectric Materials

In this study, γ-ray shielding parameters (transmission factors (TF), linear attenuation coefficients (μ), mass attenuation coefficients (μ⁄ρ), mean free path ("λ" ), radiation protection efficiency (RPE), half-value layer (HVL), and tenth value layer (TVL)) were measured of some dielectric materials (amber, plexiglass, organic glass, quartz, bakelite, NaCl, porcelain, and marble). The absorption measurements were done by EDXRFS (Energy Dispersive X-ray Fluorescence Spectrometer). The study aims to create new areas of use thanks to the measurements and calculations to be made on these technologically important dielectric materials. According to the results obtained, amber is the best gamma ray shielding material, while quartz is not suitable for gamma ray shielding.

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.

As seis pinturas de Massimo Campigli do MAC USP discutidas sob o olhar das artes plásticas e dos resultados de análises com técnicas de imagens e espectroscópicas

This article focuses on the discussion of the results obtained with non-invasive image and spectroscopic analyzes (to determine chemical elements and compounds) on the six paintings by the German artist, naturalized Italian, Massimo Campigli, that belong to the collection of the Museum of Contemporary Art of the University of São Paulo (MAC USP). Aspects of the artist’s trajectory, the plastic solutions of the artworks, along with the analyzes made with the spectroscopic techniques of energy dispersive X-ray fluorescence (ED-XRF), Raman, and Fourier transform infrared (FTIR), and the imaging techniques of visible photography (VIS), raking light (RAK), transmitted light (TRANS), visible ultraviolet fluorescence (UVF), infrared reflectography (IRR), and radiography (RAD) offer important information on the artist and on his work. These non-invasive analyzes were carried out in the museum itself with portable equipment from the Laboratory of Archaeometry and Applied Sciences to Cultural Heritage (LACAPC) of the Physics Institute (IF) of USP. Overall, the results obtained corroborate with Campigli’s testimonies about his artistic practice, as well as those of people who saw him working in his studio. His palette choice, composed by natural and synthetic pigments, mostly whites and paints with earthy tones, and his creative steps of creating and recreating the paintings, reusing canvases many times, were proven to be true with the analytical investigations.

DEVELOPMENT OF A REFERENCE SAMPLE FOR RAPID ANALYSIS OF AN ELEMENTAL COMPOSITION OF MEDICINAL PLANT RAW MATERIALS

Objective: Development and validation of a technique for preparation of a reference sample for elemental microanalysis using the XRF technique in terms of repeatability, reproducibility, and optimization of the technique for rapid determination of the elemental composition of medicinal plants based on X-ray fluorescence analysis. Methods: Samples: fresh shoots of Kalanchoe daigremontiana, ready reference sample "Birch Leaf" LB-1 (A. P. Vinogradov Institute of Geochemistry, Siberian Branch of the Russian Academy of Sciences, Irkutsk, Russia), and IAEA reference sample SRM 2976 (IAEA, MEL, Monaco). The dispersed fraction was analyzed using a Master Sizer 2000 instrument (Malvern Panalytical, Worcestershire, UK). Elemental analysis using an energy dispersive X-ray fluorescence spectrometer EDX-7000 Shimadzu (Shimadzu Corporation, Kyoto, Japan), GZ-AAS using an Agilent instrument, model 240Z AA instrument (Agilent Technologies, Inc., Santa Clara, USA) with electrothermal atomization and Zeeman background correction, and ICP-MS using an Agilent 7500 CE instrument (Agilent Technologies, Inc., Santa Clara, USA). Results: By the LALLS method, they were separated by the maximum distribution, which was 63 microns, and a minor fraction of 39 microns. This indicates sufficient homogeneity in the sample. Further, homogeneity was proved by the XRF method by measuring six independent samples obtained by the quartering method. Also, the elemental composition of the reference samples was determined: completely dried, homogenized before sifting, and homogenized after sifting. Further, the obtained reference sample of K. daigremontiana was compared with reference samples: IAEA SRM 2976 and "birch leaf methods: ICP-MS, GZ-AAS, XRF. Conclusion: The reference sample will allow for rapid analysis of medicinal plant raw materials. Standardization of medicinal plants by the content of microelements will allow observing species differences as well as adjusting the concentrations of microelements for therapeutic purposes using medicinal plants.

Elemental Composition of A Cultivated Mushroom (Agaricus bisporus) and Some Wild Mushroom Species

In the study, a cultivation mushroom (Agaricus bisporus) and some wild mushroom species (Schizophyllum commune, Pleurotus ostreatus, Lactarius deliciosus, Hebeloma sinapizans, Hygrophorus ligatus, Suillus luteus, Armillaria mellea, Coprinus comatus, Psathyrella candolleana, Russula torulosa, Trametes pubescens) were investigated in terms of elemental compositions. The wild mushroom species were collected from Trabzon province. Mg, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Rb, Sr, Y, Zr, I, Hf, Hg, Pb metal concentrations were determined using Energy Dispersive X-ray Fluorescence (ED-XRF) device. The highest aliminium, silicium, vanadium, zirconium, iron and mercury were determined in Lactarius deliciosus. The highest potassium, arsenic, rubidium, iodine contents were determined in Hebeloma sinapizans. The highest manganese, zinc, lead contents were determined in Hygrophorus ligatus. The highest magnesium, chromium, nickel, yttrium contents were determined in Coprinus comatus. The highest titanium and selenium were determined in Psathyrella candolleana. The highest calcium and strontium were determined in Russula torulosa. The highest hafnium was determined in Schizophyllum commune. The highest phosphate was determined in Agaricus bisporus. The highest sulphur was determined in Armilleria mella. The highest copper was determined in Suillus lutesus. It was concluded that elemental composition of mushrooms was affected especially by mushroom specie.