Search Results (586)

This study analyzes the durability of brick-faced clay-core walls (BCWs) in the traditional residential architecture of Quanzhou—a UNESCO World Heritage City. Taking the northern gable of Ding Gongchen’s former residence as an example, the mechanical properties, microscopic structure, and changes in chemical symbol, oxides and minerals of the red bricks and clay-cores were analyzed using finite element mechanics analysis (FEM), scanning electron microscopy (SEM), X-ray fluorescence (XRF), and X-ray diffraction (XRD). The results indicate a triple mechanism: (1) The collaborative protection and reinforcement mechanism of “brick-wrapped-clay”. (2) The infiltration and destruction mechanism of external pollutants. (3) The material stability mechanism of silicate minerals. Therefore, the key to maintaining the durability of BCWs lies in the synergistic effect of brick and clay materials and the stability of silicate mineral materials, providing theoretical and methodological support for sustainable research into brick and clay constructions. Full article

This study explored the extraction, characterization, and biological properties of polysaccharides derived from Spirulina (Limnospira platensis), a microalga known for its rich nutritional benefits. Polysaccharides were successfully isolated and characterized using optimized biorefinery water extraction techniques to detail their structural and functional characteristics. Results revealed notable antioxidant activity and effective α-glucosidase inhibition, indicating potential health benefits. X-ray fluorescence (XRF) analysis was conducted to assess the elemental composition, offering insights into the mineral contents of the polysaccharides. Our findings underscore the promising applications of polysaccharides from Limnospira platensis as functional ingredients in health-related fields, advocating the need for further research into their mechanisms of action and therapeutic applications. Full article

The most important bauxite deposits in Türkiye are located in the Seydişehir (Konya) and Akseki (Antalya) regions, situated along the western Taurus Mountain, with a total reserve of approximately 44 million tons. Some of the bauxite deposits have been exploited for alumina since the 1970s. In this study, bauxite samples, collected from six different deposits were examined to determine their mineralogical and chemical composition, as well as their REE content, with the aim of identifying which bauxite types are enriched in REEs and assessing their economic potential. The samples included massive, oolitic, and brecciated bauxite types, which were analyzed using optical microscopy, X-ray diffraction (XRD), X-ray fluorescence (XRF) and inductive coupled plasma-mass spectrometry (ICP-MS), field emission scanning electron microscopy (FESEM-EDX), and electron probe micro-analysis (EPMA). Massive bauxites were found to be more homogeneous in both mineralogical and chemical composition, predominantly composed of diaspore, boehmite, and rare gibbsite. Hematite is the most abundant iron oxide mineral in all bauxites, while goethite, rutile, and anatase occur in smaller quantities. Quartz, feldspar, kaolinite, dolomite, and pyrite were specifically determined in brecciated bauxites. Average oxide contents were determined as 52.94% Al₂O₃, 18.21% Fe₂O₃, 7.04% TiO₂, and 2.69% SiO₂. Na₂O, K₂O, and MgO values are typically below 0.5%, while CaO averages 3.54%. The total REE content of the bauxites ranged from 161 to 4072 ppm, with an average of 723 ppm. Oolitic-massive bauxites exhibit the highest REE enrichment. Cerium (Ce) was the most abundant REE, ranging from 87 to 453 ppm (avg. 218 ppm), followed by lanthanum (La), which reached up to 2561 ppm in some of the massive bauxite samples. LREEs such as La, Ce, Pr, and Nd were notably enriched compared to HREEs. The lack of a positive correlation between REEs and major element oxides, as well as with their occurrences in distinct association with Al- and Fe-oxides-hydroxides based on FESEM-EDS and EPMA analyses, suggests that the REEs are present as discrete mineral phases. Furthermore, these findings indicate that the REEs are not incorporated into the crystal structures of other minerals through isomorphic substitution or adsorption. Full article

In this study, high-energy milled (HEM) samples of natural phosphorites from Estonian deposits were investigated. The activation was performed via planetary mill with Cr-Ni grinders with a diameter of 20 mm. This method is an ecological alternative, since it eliminates the disadvantages of conventional acid methods, namely the release of gaseous and solid technogenic products. The aim of the study is to determine the changes in the structure to follow the solid-state transitions and the isomorphic substitutions in the anionic sub-lattice in the structure of the main mineral apatite in the samples from Estonia, under the influence of HEM activation. It is also interesting to investigate the influence of HEM on structural-phase transformations on the structure of impurity minerals-free calcite/dolomite, pyrite, quartz, as well as to assess their influence on the thermal behavior of the main mineral apatite. The effect of HEM is monitored by using a complex of analytical methods, such as chemical analysis, powder X-ray diffraction (PXRD), wavelength-dispersive X-ray fluorescence (WD-XRF) analysis, and Fourier-transformed infrared (FTIR) analysis. The obtained results prove the correlation in the behavior of the studied samples with regard to their quartz content and bonded or non-bonded carbonate ions. After HEM activation of the raw samples, the following is established: (i) anionic isomorphism with formation of A and A-B type carbonate-apatites and hydroxyl-fluorapatite; (ii) solid-phase synthesis of calcium orthophosphate-CaHPO₄ (monetite) and dicalcium diphosphate-β-Ca₂P₂O₇; (iii) enhanced chemical reactivity by approximately three times by increasing the solubility via HEM activation. The dry milling method used is a suitable approach for solving technological projects to improve the composition and structure of soils, increasing soil fertility by introducing soluble forms of calcium phosphates. It provides a variety of application purposes depending on the composition, impurities, and processing as a soil improver, natural mineral fertilizer, or activator. Full article

In this paper, mussel shells were used to produce chitin, chitosan, and calcium acetate using chemical processes, searching for an alternative environmentally friendly biopolymer and calcium source. Mussel shells were treated with acetic acid as a demineralizing agent, resulting in separate solid fractions and calcium solution. The solid was further purified to produce chitin by deproteinization and decolorization processes, and then the deacetylation process was used to obtain chitosan. The calcium solution was evaporated to produce calcium acetate powder. The yields of extracted chitin, chitosan, and calcium acetate from 100 g of mussel shells were 2.98, 2.70, and 165.23 g, respectively. The prepared chitin, chitosan, and calcium acetate were analyzed by Fourier transform infrared (FTIR) spectrophotometry, X-ray diffraction (XRD), thermogravimetric analysis (TGA), and scanning electron microscope (SEM) to confirm the chemical and physical properties. The analysis results of chitin and chitosan revealed the similarity to chitosan derived from crustaceans and insects in terms of functional group, structure and morphologies. The prepared calcium acetate shows FTIR and XRD data corresponding to calcium acetate monohydrate (Ca(CH₃COO)₂·H₂O) similar to synthesized calcium acetate in previous research. In addition, the mineral contents of calcium acetate identified by X-ray fluorescence (XRF) analysis exhibit 97.8% CaO with non-toxic impurities. This work demonstrated the potential of the production process of chitin, chitosan, and calcium acetate for the development of a sustainable industrial process with competitive functional performance against the commercial chitin and chitosan production process using crustacean shells and supported the implementation of a circular economy. Full article

This study investigates the influence of superabsorbent polymer (SAP) particle size on the mechanical and shrinkage behavior of concrete. Five concrete mixtures were prepared using SAPs with varying size ranges: 150–300 µm, 300–600 µm, 600–1800 µm, and a blended mix combining 300–600 µm and 600–1180 µm. The primary focus was on evaluating compressive strength, elastic modulus, autogenous shrinkage, drying shrinkage, and total shrinkage. The mechanical performance and dimensional stability were measured at different curing ages, and microstructural analysis was conducted using X-ray fluorescence (XRF) at 7 days to examine changes in chemical composition. Results showed that smaller SAP sizes contributed to more homogeneous internal curing, improved hydration, and higher matrix density. In contrast, larger SAP particles were more effective in reducing shrinkage but slightly compromised strength and stiffness. This study emphasizes the importance of selecting appropriate SAP particle sizes to balance mechanical integrity and shrinkage control, contributing to the development of high-performance concrete with reduced cracking potential. Full article

The cements industry is increasingly under pressure to reduce carbon emissions while maintaining performance standards. Limestone calcined clay cement (LC³) presents a promising low-carbon alternative; however, its performance depends significantly on the type and reactivity of clay used. This study investigates the effect of three common low-grade clay minerals—kaolinite, montmorillonite, and illite—on the behavior of LC³ blends. The clays were thermally activated and characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), X-ray fluorescence spectroscopy (XRF), and Blaine air permeability testing to evaluate their mineralogical composition, thermal behavior, chemical content, and fineness. Pozzolanic reactivity was assessed using the modified Chapelle test. Microstructural development was examined through scanning electron microscopy (SEM) of the hydrated specimens at 28 days. The results confirmed a strong correlation between clay reactivity and hydration performance. Kaolinite showed the highest reactivity and fineness, contributing to a dense microstructure with reduced portlandite and enhanced formation of calcium silicate hydrate. Montmorillonite demonstrated comparable strength and favorable hydration characteristics, while illite, though less reactive initially, showed acceptable long-term behavior. Although kaolinite delivered the best overall performance, its limited availability and higher cost suggest that montmorillonite and illite represent viable and cost-effective alternatives, particularly in regions where kaolinite is scarce. This study highlights the suitability of regionally available, low-grade clays for use in LC³ systems, supporting sustainable and economically viable cement production. Full article

This paper presents the synthesis of La₂Ti₂O₇ nanoparticles by the sol–gel method starting from lanthanum nitrate and titanium alkoxide (noted as LTA). Subsequently, the lanthanum titanium oxide nanoparticles are modified with noble metals (platinum) using the chemical impregnation method, followed by a reduction process with NaBH₄. The comparative analysis of the structure and surface characteristics of the nanopowders subjected to thermal treatment at 900 °C is conducted using Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray fluorescence (XRF), ultraviolet-visible (UV–Vis) spectroscopy, as well as specific surface area and porosity measurements. The photocatalytic activity is evaluated in the oxidative photodegradation of ethanol (CH₃CH₂OH) under simulated solar irradiation. The modified sample shows higher specific surfaces areas and improved photocatalytic properties, proving the better conversion of CH₃CH₂OH than the pure sample. The highest conversion of ethanol (29.75%) is obtained in the case of LTA-Pt after 3 h of simulated solar light irradiation. Full article

This work investigates photoactive inorganic powders (SiO₂, IrSiO₂, and IrO₂/IrSiO₂) and their derivatives modified with metallated porphyrin, focusing on their ability to generate reactive oxygen species (ROS) under visible light exposure. The core material, SiO₂, exhibits a tubular morphology and a high density of optically active defects. Modifiers such as metallic and iridium oxide nanoparticles, along with porphyrin, are employed to enhance light absorption and the generation of singlet oxygen (¹O₂) for potential biomedical applications. The time-dependent photogeneration of singlet oxygen is monitored using a Singlet Oxygen Green Sensor (SOSG), and its reactivity is evaluated in relation to DL α-Tocopherol through a spectrofluorimetric analysis. The photoactive materials, both before and after porphyrin modification, are characterized using Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), X-ray Diffraction (XRD), X-ray Fluorescence (XRF), UV–Vis Spectroscopy, X-ray Photoelectron Spectroscopy (XPS), N₂ adsorption–desorption measurements, and zeta potential measurements. Full article

The carbonate content serves as a fundamental proxy in lacustrine sediments for reconstructing palaeoclimate and environmental changes. Although multiple analytical techniques exist for its quantification, systematic comparisons between different methodologies and the precise identification of carbonate mineralogy are still needed. In this study, a 1020 cm continuous sediment core (YZH-1) from Lake Yangzong in Yunnan Province was employed. Initially, the semi-quantitative calcium (Ca) concentration was obtained via X-ray fluorescence (XRF) core scanning. Subsequently, the total inorganic carbon (TIC) content was determined using both the loss on ignition (LOI) and gasometric (GM) methods to evaluate methodological discrepancies and potential biases. Furthermore, a quantitative regression model was developed to estimate carbonate abundance based on the relationship between XRF-derived Ca data and the analytically determined carbonate content. A comparative analysis revealed a strong positive correlation (r = 0.97) between LOI and GM measurements, though LOI-derived values are systematically elevated by 2.6% on average. This overestimation likely stems from the thermal decomposition of non-carbonate minerals during LOI analysis. Conversely, GM measurements exhibit a ~5% underestimation relative to certified reference materials, attributable to instrumental limitations such as gas leakage. Strong covariation (r = 0.92) between XRF-Ca intensities and the TIC content indicates that carbonate minerals in Lake Yangzong sediments predominantly consist of calcite. A transfer function was established to convert XRF-Ca scanning data into absolute Ca concentrations, leveraging the robust Ca-TIC relationship. The proposed quantification model demonstrates high reliability when applied to standardized XRF-Ca datasets, offering a practical tool for paleolimnological studies in similar geological settings. Full article

This study examines the formation of the clay mineral simonkolleite (Skl) in bentonites contaminated with zinc(II) chloride (ZnCl₂), a process that has been little documented in heterogeneous systems such as contaminated bentonites. We explain the contamination mechanisms and provide new insights into the mineralogical, structural, and physicochemical transformations occurring within these materials. The objective, explored for the first time, was to assess how the ZnCl₂-induced mineral phase formation influences the properties of bentonites used as sealing materials, particularly regarding changes in specific surface area and porosity. Three bentonites were analyzed: Ca-bentonite from Texas (STx-1b), Na-bentonite from Wyoming (SWy-3), and Ca-bentonite from Jelsovy Potok, Slovakia (BSvk). Treatment with ZnCl₂ solution led to ion exchange and the formation of up to ~30% simonkolleite, accompanied by a concurrent decrease in montmorillonite content by 9–30%. A suite of analytical techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), X-ray fluorescence (XRF), and energy-dispersive X-ray spectroscopy (EDS), was employed to characterize these transformations. The contamination mechanism of ZnCl₂ involves an ion exchange of Zn²⁺ within the montmorillonite structure, the partial degradation of specific montmorillonite phases, and the formation of a secondary phase, simonkolleite. These transformations caused a ~50% decrease in specific surface area and porosity as measured by the Brunauer–Emmett–Teller (BET) nitrogen adsorption and Barrett–Joyner–Halenda (BJH) methods. The findings raise concerns regarding the long-term performance of bentonite-based barriers. Further research should evaluate hydraulic conductivity, mechanical strength, and the design of modified bentonite materials with improved resistance to Zn-induced alterations. Full article

The aim of this study is to determine the characteristics of the chemical and mineral composition of sediment layers in a technogenic settling pond. This pond is located on urban land in Berezniki (Perm Krai, Russia), outside the territory of operating industrial facilities, and contains alkaline saline industrial wastes. The origin of this waste was related to sludge from the Solvay soda production process, which had been deposited in this pond over a long period of time. However, along with the soda waste, the pond also received wastewater from other industries. As a result, the accumulated sediment is characterized by variation in morphological properties both in depth and laterally. Five undisturbed columns were taken to study the composition of the accumulated sediment. The obtained samples were analyzed by X-ray diffraction (XRD), synchronous thermal analysis (STA), and X-ray fluorescence (XRF) analysis. The results showed that the mineral composition of bottom sediments in each layer of all studied columns is characterized by the predominance of calcite precipitated from wastewater. Along with calcite, due to the presence of magnesium and sodium in the solution, other carbonates precipitated—dolomite and soda (natron), as well as complex transitional carbonate phases (northupite and trona). Together with carbonate minerals, the chloride salts halite and sylvin, sulfate minerals gypsum and bassanite, and pyrite and nugget sulfur were established. The group of terrigenous mineral components is represented by quartz, feldspars, and aluminosilicates. The chemical composition of sediments in the upper part of the section generally corresponds to the mineral composition. In the lower sediment layers, the role of amorphous phase and non-mineral compounds increased, which was determined by the results of thermal analysis. The content of heavy metals and metalloids also increases in the middle and lower sediment layers. When categorized according to the Igeo value, an excessive degree of contamination (class 6) was observed in all investigated columns for copper content (Igeo 5.2–6.1). Chromium content corresponds to class 5 (Igeo 4.1–4.6), antimony to class 4 (Igeo 3.0–4.0), and lead, arsenic, and vanadium to classes 2 and 3 (moderately polluted and highly polluted). The data obtained on variations in the mineral and chemical composition of sediments represent the initial information for the selection of methods of accumulated waste management. Full article

A series of 11 Byzantine gold coins were investigated, including two examples of an extremely rare type called histamenon “stellatus”, from around the reign of the Byzantine emperor Constantine IX Monomachos (AD 1042–1055). The methods applied were X-ray fluorescence spectroscopy (XRF), specific density measurement (SD), and scanning electron microscopy (SEM). The debasement (decreasing gold content) of the Byzantine nomisma gold coinage during the 11th century was demonstrated. A method combining XRF and SD measurement combined with a graphical presentation/analysis called a ternary plot was also demonstrated. The measured gold content of the 11 coins was corrected for the possible “outwashing” effect and a potential cleaning of ancient gold. A model for the estimation of the gold content of Byzantine histamenon nomisma gold coins from the period AD 1020–1118, based on the specific density (SD), was derived. It was demonstrated that two analyzed histamenon “stellati” coins likely were minted around AD 1054–1055, possibly during the same period as the occurrence of the supernova SN1054, known as the Crab-nebula. It is further discussed if the gold content and size of the stars shown on those coins can be correlated to the visibility of the supernova from June AD 1054 to January AD 1055. Full article

Cementing operations are among the most critical steps in oil-well construction. When performed improperly, the integrity and useful life of the well can be significantly compromised. Light cement pastes are used to cement formations with a low fracture gradient to ensure zonal isolation and maintain the integrity of the casing. Extenders are additives used to reduce the density of cement pastes, ensuring that the paste has desirable properties before and after setting. This work aimed to evaluate the application of palygorskite clay as an additive in lightweight cement pastes for oil wells, highlighting how its fibrous morphology influences the microstructure and enhances the macroscopic properties of the hardened cement matrix. For this, the clay sample was initially characterized regarding its physicochemical properties using X-ray diffraction (XRD), X-ray fluorescence (XRF), thermogravimetry (TG), textural analysis (BET/N₂), and scanning electron microscopy (SEM). Lightweight pastes (1.56 g/cm³) were then formulated, varying the clay concentration by 1%, 3%, and 6% of the total mass. Cement pastes using bentonite were also formulated for comparison. Technological tests of atmospheric consistency, rheological behavior, free water, and stability were applied. It can be noted that the pastes formulated with palygorskite had lower viscosity, reflected in the reduced plastic viscosity and yield stress values, indicating easier flow behavior when compared with bentonite-based pastes. The pastes formulated with 6% palygorskite and 3% bentonite showed satisfactory stability and drawdown results. Therefore, applying palygorskite satisfies the minimum requirements for acting as an extending agent for lightweight cement pastes and is an option for application in oil-well cementing operations. Full article

This study systematically analyzes the composition and microstructure of Neolithic pottery unearthed from the Dazhuzhuang, Likou, and Biting Sites in the Yongcheng District using techniques such as X-ray fluorescence spectroscopy (XRF), X-ray diffraction (XRD), infrared spectroscopy (IR), and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS). The results show that although the raw materials for pottery at the three sites were likely sourced from nearby ancient soil layers, significant differences in chemical composition and manufacturing techniques are evident. Pottery from the Dazhuzhuang Site is mainly composed of argillaceous gray pottery, with relatively loose raw material selection and a wide fluctuation in SiO₂ content (64.98–71.07%), reflecting diversity in raw material sources. At the Likou Site, argillaceous black pottery predominates, characterized by higher Al₂O₃ content (17.78%) and significant fluctuations in CaO content (1.46–2.22%), suggesting the addition of calcareous fluxes and the adoption of standardized manufacturing techniques. Pottery from the Biting Site mainly consists of argillaceous gray pottery, showing higher Al₂O₃ content (17.36%), stable SiO₂ content (65.19–69.01%), and the lowest CaO content (0.84–1.81%). The microstructural analysis further reveals that the black pottery (from the Likou Site) displays dense vitrified regions and localized iron enrichment. In contrast, the gray pottery (from the Dazhuzhuang and Biting Sites) shows clay platelet structures and vessel-type-specific differences in porosity. This research provides important scientific evidence for understanding raw material selection, manufacturing techniques, and regional cultural interactions in the Yongcheng area during the Longshan Culture period. Full article