Energy Dispersive X-ray Fluorescence Research Articles

Assessment of Human Health Risk Caused by Heavy Metals in Kiln Dust from Coal-Fired Clay Brick Factories in Türkiye

AbstractHeavy metal (HM) pollution from natural processes and different anthropogenic activities pose significant human and environmental health risks because of their stability, non-degradable properties, and high toxicity. HM released into the air in the form of dust can enter the human body via ingestion, inhalation, and dermal contact. Keeping in mind the significance of estimating the risk from HM in different environments, the carcinogenic and non-carcinogenic health risks to workers caused by HM in kiln dust (KD) samples collected from coal-fired clay brick factories in the Western Black Sea Region of Türkiye were assessed for the first time in this study. The concentrations of major and minor oxides and HMs in the collected KD samples were analyzed using energy-dispersive X-ray fluorescence spectrometry. The average concentrations of Fe, Mn, Cr, Ni, V, Zn, Cu, As, Co and Pb analyzed in thirty-three KD samples were determined as 65444, 768, 251, 249, 248, 122, 60, 52, 42 and 16 mg/kg dw, respectively. The average levels of Ni, As, Cr, Co and Cu exceed the maximum contaminant levels recommended in the Turkish Regulation on Control of Soil Pollution. Carcinogenic and non-carcinogenic human health risk assessments for workers via three exposure pathways were carried out, estimating the hazard index (HI) and total carcinogenic risk (TCR) index, respectively. The HI values (< 1) revealed no possible non-carcinogenic health risk due to exposure to all HMs in the studied KD samples. The average TCR value revealed that the potential cancer risks for Ni, As, Cr, and Pb were slightly above the safe limit and required monitoring and further investigation for these HMs.

Physicochemical and phytochemical characterization of opuntia dillenii: A promising source of bioactive compounds

ABSTRACT The objective of this ongoing research is to investigate and assess the aqueous extracts, vegetable oil, and residual plant components derived from O. dillenii by use of HPLC, and GC-MS. Subsequent investigations employed colorimetric techniques to identify reducing and soluble sugars. We developed and validated an energy-dispersive X-ray fluorescence (EDXRF) method for determining the concentrations of essential chemical elements (O, C, Ca, Mg, K, S, P) in seeds, juice, and peel, as well as their residues. HPLC analysis yielded results indicating that extracts from O. dillenii seeds, juice, and peel from distinct regions (Oujda, Nador, and Essaouira) contained elevated concentrations of metabolites. Specifically, peel and juice extracts exhibited the highest levels of organic acids and betanin compared to O. dillenii seeds. Conversely, seed oils displayed a noteworthy tocopherol content, predominantly δ-tocopherol. Similarly, an examination of organic acid composition in juice, peel, and seeds from three different regions revealed their elevated levels. Citric acid and oxalic acid emerged as predominant components in the juice. Overall, Opuntia dillenii’s physicochemical and phytochemical characterization improves in understanding its potential as a bioactive chemical promoter, which could lead to the creation of new medicinal medicines or functional food ingredients.

Synergistic effects of zinc and cadmium on phytoremediation potential of Christmas moss (Vesicularia montagnei)

The hyperaccumulation potential of zinc (Zn) and cadmium (Cd) and their synergistic effects were examined in relation to Christmas moss (Vesicularia montagnei (Bél) Broth., Hypnaceae), an aquatic and terrestrial moss, dosed with Cd (Cd1 and Cd2), Zn (Zn1 and Zn2) and combined Zn and Cd (Cd1Zn1 and Cd2Zn2). Zinc promoted plant growth and development, particularly in the highest Zn and combined Zn/Cd treatments (Zn2 and Cd2Zn2). The Zn treatment resulted in substantial moss chlorophyll content and highest percentage relative growth rate in biomass value (0.23 mg L−1 and 106.8%, respectively); however, the Cd2Zn2 treatment achieved maximal production of chlorophyll a and total chlorophyll (0.29 and 0.51 mg L−1, respectively) due to synergistic effects. These findings suggest that Christmas moss is a highly metal-tolerant and adaptable bryophyte species. Zinc was essential for reducing the detrimental effects of Cd while simultaneously promoting moss growth and biomass development. Furthermore, Christmas moss exhibited hyperaccumulation potential for Cd and Zn in the Cd2Zn2 and Zn alone treatments, as evidenced by highest Cd and Zn values in gametophores (1002 and 18,596 mg per colony volume, respectively). Using energy dispersive X-ray fluorescence (EDXRF) spectrometry, atomic percentages of element concentrations in moss gametophores in the Zn2, Cd2 and combined Zn/Cd treatments were generally in the order: K > Ca > P > Zn > Cd. When comparing the atomic percentages of Zn and Cd in gametophores, it is likely that the higher atomic percentage of Zn was because this element is essential for plant growth and development.

Elemental profiling of agricultural soil in Hoshiarpur utilizing analytical techniques.

Our study aimed to assess the soil quality in Punjab's Hoshiarpur district through a meticulous analysis of nutrient and elemental composition. Using a variety of analytical techniques, including Neutron Activation Analysis (NAA), external Particle-induced Gamma-ray Emission (PIGE) an Ion beam analysis Technique, and energy-dispersive X-ray fluorescence (ED-XRF), we delved into soil characterization for 22 agricultural soil samples in the Punjab region. Within the NAA framework, utilizing the Pneumatic Carrier Facility and the self-serve facility at Dhruva reactor in Mumbai, a brief 1-min irradiation procedure identified pivotal elements-Na, Mg, V, Al, Mn, and K. Conversely, an extended neutron irradiation process of approximately 4h within the self-serve facility enabled the estimation of nearly 12 elements, including Rare Earth Elements (REEs), Transition elements, and other significant elements. The external PIGE technique quantified low Z elements (Na, Mg, Al, and Si), contributing to our analytical arsenal. Rigorously validating both NAA and PIGE methodologies, we compared results meticulously against established geological standard reference materials-specifically USGS RGM-1 and USGS AGV-1.Instrumental in elemental analysis, ED-XRF spectroscopy fortified our investigative endeavors by quick assessment of ten crucial elements. The elemental analysis revealed notable accumulations of Mn and Zn in the soil, surpassing the suggested permissible limits, whereas Co, Cr, and Pb were found to be within the recommended thresholds set by WHO/UNEP. Beyond elemental profiling, our study extended to estimate the accumulation levels of various elements utilizing ecological risk factors such as Contamination Factor, Potential Ecological Risk Index, Pollution Load Index, and Geoaccumulation Factor. Our findings highlighted significant accumulation of REEs including La, Sm and Yb.. This evaluation sheds new light on the interplay between soil composition and environmental health, emphasizing the need for advanced accessible agricultural technologies to prevent and forecast contaminant discharge in arable soil. This commitment aligns with our broader goal of advancing sustainable practices in soil management.

Comparison of Quantitative and Qualitative EDXRF Analysis for Provenance Study of Archaeological Ceramics

The most common scientific analysis of archaeological ceramics aims to determine the raw material source and/or production technology. Scientists and archaeologists widely use XRF-based techniques as a tool in a provenance study. After conducting XRF analysis, the results are often analyzed using multivariate analysis in addition to interpretation and conclusions. Various multivariate techniques have already been applied in archaeological ceramics provenance studies to reveal different raw material sources, identify imported pieces, or determine different production recipes. This study aims to evaluate the results of multivariate analysis in the provenance study of ceramics that belong to three cultures that settled in the same area during various prehistoric periods. Portable energy-dispersive X-ray fluorescence spectrometry (pEDXRF) was used to determine the elemental composition of the ceramic material. The ceramic material was prepared in two different ways. The ceramic body material was ground into powder, homogenized, and then pressed into tablets. After that, the same fragments are polished in suitable places. Quantitative and qualitative analyses were performed on the tablets and polished pieces. The results were subjected to both unsupervised and supervised multivariate analysis. Based on the results, it was concluded that qualitative analysis of the well-prepared shards’ surface using EDXRF spectrometry could be utilized in provenance studies, even when the ceramic assemblages were made of similar raw materials.

Ecotoxicological assessment of nano-remediated crude oil contaminated soil using Zea mays

The germination of seedlings is hindered in soil due to the excessive presence of petroleum hydrocarbons resulting from crude oil spill. This contamination not only pollutes the environment but also renders it unsuitable for habitation, inhibits animal grazing, and results in the degradation of natural beauty and aesthetic appeal. In this work, the ecotoxicological effect of nanoremediated soil previously contaminated with crude oil was assessed. Petroleum hydrocarbons were eliminated from crude oil contaminated soil through the utilization of nanomaterial adsorbents namely: Multiwalled Carbon Nanotubes (MWCNTs), MWCNTs + IONP (Iron Oxide Nanoparticle), and P.N.C (Polymer Nanocomposite) followed by the cultivation of Zea mays seedling on the nanoremediated soils then observed over a period of seven days. Both the contaminated and treated samples were evaluated for their respective functional groups, structural morphology and elemental compositions using Fourier Transform Infrared (FTIR), Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Fluorescence (ED XRF) techniques. The seedlings were then harvested, and the lengths of their leaves, shoots, and roots were measured and recorded. Results indicated a germination rate of over 70 % achieved for seedlings cultivated in the nanoremediated soils, in contrast to a germination rate of only 40 % for seedlings grown in untreated crude oil contaminated soil. Seedlings from the soil treated with P.N.C exhibited the most favorable growth parameters, with leaf, shoot, and root lengths measuring 7.64, 4.83, and 8.04 cm respectively. In comparison, seedlings germinated in crude oil contaminated soil displayed measurements of 3.4, 2.79, and 5.32 cm for leaf, shoot, and root lengths, respectively. The pH levels of the treated soils were raised from 5.7 to 6.9, 6.3, and 6.7 for MWCNTs only, MWCNTs + IONP, and P.N.C, respectively. This augmentation had a positive impact on the uptake of nutrients through the root hairs. Additionally, it was noted that the presence of MWCNTs did not impede the germination and growth of Zea mays seedlings. This technique exhibits considerable potential for widespread adoption by farmers, oil companies, and environmental agencies as a rapid and effective nano-remediation method.

Effect of Soil Tillage Systems and Crop Seasonality on the Sediment Geochemical Properties Transferred into a Headwater: A Case of Study in Tobacco Plantation

ABSTRACT The global impacts of agricultural land conversion on soil erosion and pollution, particularly in tobacco cultivation areas, are well-recognized as significant contributors to soil degradation. These areas are identified as hotspots for environmental concerns due to practices that lead to increased erosion and pollution. From this perspective, this case of study explores fine sediment samples from two areas with tobacco cultivation under different tillage systems and seasonal variations, transport into a headwater, and evaluates, on a local scale: (1) the impact of tillage systems on the geochemical signature of sediments; (2) if whether crop seasonality affects these sediment geochemical signatures. The Conventional Ridge Tillage (CRT) system involves extensive soil exposure and machinery for soil management, while the Mulch Ridge Tillage (MRT) system prioritizes soil conservation and relies on herbicides for weed control. The analytical methodology used to assess the sample element characteristics was Energy Dispersive X-ray Fluorescence (EDXRF). It was applied on the twenty fine sediments (ten of harvest and ten of inter-harvest season of tobacco) to quantitatively assess their inorganic composition. Additionally, Pearson correlation analysis, Hierarchical Cluster Analysis (HCA), and Principal Component Analysis (PCA) were applied on the EDXRF data to highlight the similarities and, thus, providing information to assess the complex data clustering patterns. As a result, the sediment compositions from the two studied soil systems are not similar. The PCA showed that the CRT sediments are characterized by the P, S, K, Ca, and Mn content, presenting a geochemical signature related to manure and fertilizer compared to the MRT, which is correlated with Al, Ti, Fe, Cu, and Zn contents, exhibiting a geochemical signature characterized by the natural soil composition. Therefore, the sediment geochemical signatures might be affected by two phases in the study area: a) tillage system characteristics and b) seasonal soil erosion. These findings underscore the importance of managing soil nutrients to mitigate soil pollution and nutrient exportation to aquatic systems. Moreover, the results emphasize the recommendations for sustainable agricultural practices in tobacco-growing areas to protect environmental quality.

Reversible Hydrophobic Deep Eutectic Solvent-Based Uranyl-Sensing Optode Film in Aqueous Streams: Color Transformation and Reusability.

A hydrophobic deep eutectic solvent (HDES)-based optode was designed for the preconcentration and determination of the UO22+ ion in aqueous media using spectroscopic techniques [energy-dispersive X-ray fluorescence (EDXRF) and solid-state absorption]. The optode was developed by incorporation of HDES (tri-n-octyl phosphine oxide and decanoic acid in an equimolar ratio), tri-(2-ethylhexyl) phosphate, and 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol into a cellulose triacetate matrix. Characterization studies were carried out using different techniques to understand the roles of HDES as a plasticizer, UO22+ extractant, and Br-PADAP immobilizer. Uptake studies revealed that the optimal pH was 3 and sorption followed the type II adsorption isotherm. Uranium in the U-sorbed optode can be directly analyzed over a large concentration range of 0.021 × 10-3-2.1 × 10-3 Mol L-1 using EDXRF. The optode film exhibited a linear dynamic range of 0.84 × 10-6-84 × 10-6 Mol L-1 for uranium, with a lowest limit of detection of 0.084 × 10-6 Mol L-1 by colorimetric analysis. This optode-based method was employed for seawater analysis for its UO22+ concentration without any matrix separation, and the concentration was found to be 1.30 ± 0.06 × 10-8 Mol L-1. The optode exhibited better selectivity for UO22+ in the presence of various cations including Sr2+ and Cs+ in an aqueous medium. Compared to other prevailing optical sensors, this optode performed better in terms of key factors like pH, equilibration time, reusability, and detection limit.

Development of δ-Bi2O3/Bi2SiO5 heterostructures based on biogenic silica for photocatalytic treatment from organic pollutants

ABSTRACT δ-Bi2O3/Bi2SiO5 heterostructural photocatalysts with different contents of bismuth in samples (X-Bi-Si, where X = 10–60% Bi2O3) were prepared by the facile sol–gel method using bismuth nitrate and biogenic silica from rice husk biomass as precursors. FT-IR, scanning electron microscope, XRD, energy-dispersive X-ray fluorescence, and UV–Vis methods were systematically used to characterize the as-obtained materials. The photodegradation of methyl orange (MO) in neutral aqueous solutions (pH (6.8)) under UV irradiation was studied to evaluate their photocatalytic activities. The phase composition, morphology, and photocatalytic activity of the samples depended on the content of bismuth oxide in the samples. The maximum degree of MO degradation was 45% for 50-Bi-Si samples containing photoactive δ-Bi2O3 and Bi2SiO5 phases.

Anatomy of the Painting: The Study of the Serbian Orthodox Icon from the Turn of the Seventeenth to the Eighteenth Century

The paper presents the results of the multi-analytical study of the painting on a panel from the icon collection of the Gallery of Matica srpska museum in Novi Sad, Serbia. It is part of the research aiming to set the methodology for the museum’s database on artistic materials and techniques present in the collection. Computer tomography (CT) scanning was used to understand the structure of the wooden panel support. Ultraviolet (UV) and infrared (IC) imaging, as well as visible (VIS) macro photography, were used to study the paint layer, both the original part and restoration treatments, as well as the coat of varnish. Energy dispersive X-ray fluorescence (EDXRF) and Fourier-transform infrared (FTIR) spectroscopy revealed the pigments, binders, and metal leaf, defining the artistic technique. Optical microscopy (OM) and scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS) were used to disclose the stratigraphy and composition of layers in the artwork. The multi-analytical approach confirmed that protein-based binder, gilding, silver leaf, and traditional pigments were used. The data gathered from this research are important for studying the artistic materials and techniques in icon production and defining the methodology setting for the museum collection’s databases as the reference material.

Radiation shielding parameterizations of FeSO4, CuSO4, NiSO4 and ZnSO4 Compounds: using (XRF) technique & Monte Carlo FLUKA approach

The mass attenuation coefficient (MAC) for different sulphate compounds can be estimated by using the Energy Dispersive X-ray Fluorescence (EDXRF), also known as X-ray Fluorescence (XRF) technique. The X-ray photons emitted have different energies depending on incident photon energy, atomic weight, and molecular structure of tested material. The excitation energy of the gamma rays source with 59.53 keV was obtained by using 241Am (40 µci). The (MAC) for sulphate compounds of a different element (Fe, Ni, Cu, Zn) have been calculated by measuring the intensity difference for kα in pure elements and their compounds. The determined results showed that the maximum value for (µm) was in FeSO4. These results are consistent with the theoretical value obtained by the XCOM software in addition to investigating the wide energy response of photon interaction with the introduced compounds using the FLUKA Monte Carlo simulation software. The mass attenuation coefficient (MAC) of these compounds is numerically evaluated in the energy range 0.015-15 MeV using the FLAIR code. The computed (µm) is used to generate significant radiation protection factors such as the linear attenuation coefficient (LAC), half-layer value (HVL), effective (Zeff), and equivalent (Zeq) atomic number. For studying the shielding effectiveness and efficiency, for fast and thermal neutron radiation, the removal cross-section ƩR was given.

Unexplored catalytic potency of a magnetic CoFe2O4/Ni-BDC MOF composite for the one-pot sustainable synthesis of 5-substituted 1-H tetrazoles

Within the domain of materials science and engineering, significant progress has led to the emergence of innovative materials based on magnetic MOFs, positioning them as promising candidates in the field of catalysis. This research aims to elaborate on the development of a finely tailored magnetic MOF composite; Ni-BDC (Nickel benzene-1,4-dicarboxylate) microflakes which was synthesized through a straightforward in-situ solvothermal approach. Extensive investigations into the structural properties of the resultant hybrid composite were carried out using various characterization techniques encompassing X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET) analysis, atomic absorption spectroscopy (AAS), energy-dispersive X-ray spectroscopy (EDX), energy-dispersive X-ray fluorescence (ED-XRF), and vibrating sample magnetometry (VSM). The developed material demonstrated remarkable efficiency in expediting the synthesis of a diverse array of pharmaceutically active 5-substituted 1H-tetrazole derivatives through a multicomponent coupling reaction involving substituted aldehydes, malononitrile, and sodium azide as key components. A noteworthy feature of this approach is its adherence to environmentally friendly reaction conditions, thus making it superior in comparison to previously established methodologies. Furthermore, a plausible mechanistic pathway has been proposed to elucidate the impressive performance of the developed catalytic system in the targeted reaction. It is anticipated that the current research will not only contribute to the purposeful designing of advanced magnetic MOF-based architectures but will also play a pivotal role in promoting sustainable practices in industrial processes, addressing pressing environmental and economic concerns.

Adsorption of Cu(II) and Zn(II) onto ZrO2–SiO2 composite: Characteristics, mechanism and application in wastewater treatment

The presented paper describes a perspective methodology of hazardous post-production wastewater treatment focused on recovering selected metal ions species, mainly copper, zinc, and arsenic. The idea included the design of multifunctional adsorbents composed of zirconia and silica, their physicochemical evaluations, and verification tests in the adsorption process performed using model wastewaters. The proposed synthesis protocol allowed to obtain the materials with unique structural and physicochemical properties, including well-developed surface area (ABET = 398 m2∙g−1), as well as specific surface nature. It was confirmed by the results of energy dispersive X-ray, X-ray fluorescence and Fourier transform infrared spectroscopy analyses. Furthermore, by analysing the batch experiments, optimal process parameters for recovering the analyzed metal ions were established as follows: T = 313 K, pH = 5, S:L ratio = 6.67 mg:cm3, and t = 120 min. It was found that the performed removal of selected metal ion species followed pseudo-second-order kinetic and Langmuir isotherm models, and the estimated sorption capacity of the designed material was 23.5 mg∙g−1 and 12.4 mg∙g−1 for Cu(II) and Zn(II) ions, respectively. The results indicate that it is possible to separate arsenic compounds from copper and zinc ions with efficiencies of 98.9 % and 99.5 % respectively.

Insights of the adsorption mechanism of Bemacid Red using coagulation-flocculation sludge: Optimisation using BBD-RSM and DFT calculations

This study optimized the adsorption parameters for removing Bemacid Red dye using biochar derived from coagulation-flocculation sludge. The biochar was comprehensively characterized by X-ray diffraction, Fourier-transform infrared spectroscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy, thermogravimetric analysis, X-ray fluorescence, and point of zero charge determination. Adsorption experiments were conducted by varying the adsorbent dose, temperature, contact time, and initial dye concentration. A Box-Behnken design with response surface methodology was used to optimize the conditions. The experimental results closely matched the model predictions. The analysis of variance validated the model. The optimum conditions were 1.2 g. L−1, 45 °C, 40 min, and 80 mg. L−1 initial concentration, achieving 97.27 % removal efficiency. B3LYP/6-31G(d) quantum calculations supported the results. Global reactivity descriptors and local Fukui indices were calculated to elucidate adsorption mechanisms. This study highlights the effectiveness of low-cost coagulation sludge biochar for removing dyes from textile wastewater and provides a comprehensive understanding of the adsorption process through experimental and theoretical approaches.

Colouring mechanism and firing technology of white porcelain from the Sui Dynasty (581–618) from the Xiangzhou kiln, Anyang, China

The Xiangzhou kiln was one of the first significant kilns in China to fire white porcelain and as well as the earliest one to adopt the technique of Make-up clay. It plays a very important role in the history of Chinese ceramics. Here we utilize ten pieces of Sui (581–618) white porcelain from the Xiangzhou kiln as the research objects. The chemical composition, micro-morphology, firing temperature, firing atmosphere, micro-area composition and other characteristics of white porcelain glaze were tested by energy dispersive X-ray fluorescence spectroscopy (EDXRF), laser Raman spectroscopy (LRS), optical microscope (OM), thermal dilatometer (TD), focused ion beam scanning electron microscope combined with X-ray energy spectrometer (SEM-EDS), X-ray photoelectron spectroscopy (XPS) and spectrophotometer (UV–Vis–NIR). Finally, the firing technology and colouring mechanism of the Xiangzhou white porcelain are revealed. Our study demonstrates that the relatively high content of Fe2O3 and TiO2 in the white porcelain glaze of the Xiangzhou kiln results in a milky white glaze with a slight greenish tinge. The high content of CaO and K2O in the glaze and the almost entirely glass phase of glaze layer lead to the fine grain, good transparency and gloss. Most of the white porcelain of the Xiangzhou kiln is fired at high temperature under reducing atmosphere. The Xiangzhou kiln white porcelain glaze belongs to the crystalline glaze, glaze disorderly distribution of some calcium feldspar precipitation crystals and a very small amount of quartz, calcite residual crystals, glaze bubbles are larger, the distribution of relatively dispersed. The overall colour effect of the Xiangzhou kiln white porcelain results from the combined action of the chemical colour of the body and glaze, along with structural colour.

Profile of mineral nutrients and proteins in soybean seeds (Glycine max (L.) Merrill): Insights from 95 varieties cultivated in Brazil

Soybean (Glycine max (L.) Merrill) stands out as a major source of protein meal for human and animal nutrition. Nevertheless, the increase in soybean yield has been accompanied by a reduction in protein content over the last decades. In this study, we determined the profile of mineral nutrients and total protein in 95 soybean varieties broadly cultivated in Brazil, the world’s largest soybean producer and exporter, to identify a possible association between seed mineral and protein content. Energy-dispersive X-ray fluorescence spectroscopy (EDXRF) was employed to determine the concentration of macro, i.e., potassium (K), phosphorus (P), sulphur (S), calcium (Ca), and micronutrients, i.e., iron (Fe), manganese (Mn), zinc (Zn), and copper (Cu). The protein content of soybean seeds was evaluated using the Dumas method. The correlation and clustering between nutrients and proteins were determined using both univariate and multivariate non-parametric tests. Both protein and nutrient concentrations were not homogeneous across soybean seed varieties. It was also revealed that the higher the seed protein content, the higher the S, Mn, and Zn concentrations, whereas the opposite trend was observed for K and P. These results indicate an intricate association between S, Zn, Mn, and total protein content in soybean seeds.

Minimum Spanning Tree‐Based Clustering for Chemical Evaluation of Commercial Nail Polish Samples Using Spectroanalytical Data

ABSTRACTThis study discusses potential toxic elements detection in conventional nail polish, including Cr and Pb. The noteworthy results highlight well‐established potential risks of elevated Cr and Pb concentrations. These elements are not allowed in the European Union. Implementing the minimum spanning tree (MST) approach and the isolation forest algorithm effectively clustered samples. Forty‐five samples were analyzed, and four clusters were identified. Two presented six samples with high concentrations of Fe (Cluster 1 with four samples) and Cr and Pb (Cluster 2 with two samples). The other 39 samples presented low concentrations of the determined elements (Co, Cr, Cu, Fe, Ni, and Pb). Cadmium, Zn, and Mn were not detected in any of the analyzed samples. Furthermore, integrating energy‐dispersive x‐ray fluorescence (ED‐XRF) and laser‐induced breakdown spectroscopy (LIBS) enabled fast direct analysis of nail polish samples, streamlining a swift and reliable data acquisition process. This research underscores the importance of ongoing vigilance and monitoring of potential health hazards associated with nail polish formulations, especially in regions with regulatory restrictions on certain elements.

Features of the iron determination in dust emissions of gas purification of electrometallurgical production

Features of the iron determination in dust emissions of gas purification at electrometallurgical facilities are considered. The elemental and phase compositions of dust emissions were determined using energy dispersive x-ray fluorescence analysis (EDXRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Sample preparation conditions were optimized with allowance for the analytical methods used. The phase composition of dust emissions represented mainly by zincite, zinc ferrite, halite and sylvite was preliminary determined by X-ray phase analysis. Model mixtures were prepared and used to construct calibration dependences taking into account the results of diffractometric studies. A technique for rapid x-ray fluorescence determination of iron in dust emissions of gas purification has been developed. The methods for iron determination tested on real samples of dust emissions of electrometallurgical production demonstrated a satisfactory convergence of the results obtained by EDXRF (Sr = 1.3%) and ICP-AES (Sr = 2.6%).

The Iridescent Painting Palette of Michelino da Besozzo: First Results of Non-Invasive Diagnostic Analyses

This study concerns the characterization of the color palette of Michelino da Besozzo, one of the leading painters and illuminators of the Late Gothic period in Northern Italy. The artist’s relationship with the color blue was investigated by considering the recipe for lapis lazuli given by the artist to Giovanni Alcherio in Venice in 1410 and found in the medieval treatise of Jean Lebegue. The paper highlights this important evidence for the study of painting technique in the first half of the 15th century with an analytical and technical study of two paintings: The Mystic Marriage of Saint Catherine (Siena, Pinacoteca Nazionale, inv. 171) and The Madonna of the Rose Garden (Verona, Museo di Castelvecchio, inv. 173-1B359). These two case studies were approached through analyses carried out with non-invasive and portable techniques such as Energy Dispersive X-ray Fluorescence (ED-XRF) spectroscopy and Fiber Optics Reflectance Spectroscopy (FORS). The results show a color palette based on ultramarine, azurite, verdigris or copper resinate; earths, cinnabar or vermillion; and lead white, yellow and red ochre and lac. These preliminary results made it possible to clarify certain aspects of the artist’s style and his painting technique and identify common elements between the two works of art.

Mineral and particle-size chemometric classification using handheld near-infrared instruments for soil in Northeast Brazil

The characterization of soil variations crucial for agriculture is challenging due to soil having different mineral composition and particle-size distribution. Traditional methods are costly and time-consuming for large-sized areas. Spectroscopic techniques coupled with chemometrics are alternative ways to overcome these drawbacks. Miniaturized near-infrared (NIR) spectrophotometers provide fast, cost-effective spectra acquisition for assessing soil chemistry and distribution despite challenges like overlapped bands and reduced spectral range. This study presents a pattern recognition strategy to address these limitations, enhancing the use of handheld NIR instruments for soil analysis. The study analyzed 176 soil samples from 15 soil groups in the Northeast region of Brazil. First, attenuated total reflectance-Fourier transform infrared (ATR-FTIR) and energy-dispersive X-ray fluorescence spectrometry (EDXRF) were employed to characterize the samples, providing complementary vibrational and elemental information, respectively. Common Dimension Analysis (ComDim) identified links between ATR-FTIR and EDXRF data, aiding soil characterization. The Common Components (CCs) from ComDim were used in Partitioning Around Medoids (PAM) clustering, resulting in five distinct classes based on their mineral composition. These classes showed significant differences in clay and sand contents. With the use of ComDim-PAM, samples were labeled for classification via Partial-least Squares-Discriminant Analysis (PLS-DA) and Support Vector Machine (SVM) using NIR spectra (spectral range: 908–1676 nm) from two handheld instruments (Hand 1 and Hand 2). The SVM models outperformed the PLS-DA models, especially by including variable selection for Hand 1, with test accuracy exceeding 90%. These findings highlight the method's advantages for fast and cost-effective assessment, classification, and soil mapping based on their mineral and particle-size distribution.