X-ray Fluorescence Spectrometry Research Articles

A Typology and Lead Isotope and Cultural Exchange Study on Bronze Knives from Shuangyuan Cemetery, Chengdu City, Southwest China

Background: Bronze knives, which have been excavated in large quantities and acquired hierarchical significance, are essential artifacts in Shu State in Southwest China. Building upon previous typological analyses of bronze knives, it is hypothesized that Shu culture may have imported foreign-style bronze knives. However, further demonstration of the provenance of metal materials, the typology of knives, and the cultural exchange necessitates a comprehensive examination through the lens of scientific analysis. The purpose of this study is to investigate the differences in the manufacturing processes and metal resources of Shu bronze knives with various cultural styles and whether bronze knives in the foreign styles were imported or locally imitated. Methods: In this study, the typology, portable X-ray fluorescence spectrometry and multi-collector inductively coupled plasma mass spectrometry were used to analyze twenty-four bronze knives unearthed from Shuangyuan cemetery, a cemetery of the Eastern Zhou Dynasty in Chengdu City, Sichuan Province, Southwest China. Results: The results of the study show that the knives of Shuangyuan Cemetery can be classified typologically into five types, encompassing both local and foreign styles. The predominant alloy composition of these knives is lead-tin bronze, characterized by a notably high tin content. Lead isotope ratios indicate that metal materials from the South China geochemical province and Yangtze geochemical province were mainly used to manufacture the bronze knives unearthed from the Shu state Conclusion: While the majority of foreign-style knives with ring-shaped heads were likely imported from neighboring regions like Chu state, distinctively styled type D and type E bronze knives appear to have been locally imitated by the Shu, showcasing a blend of external influences and indigenous innovation. The combination of typology and scientific analysis of the bronze knife may shed new light on the study of the Shu culture of the Eastern Zhou period.

Heat-resistant concretes based on cement binders and waste from the metallurgical industry

The main direction of the development of heat-resistant concrete production is the use of new materials, ensuring mechanization and industrialization of construction, increasing the performance characteristics of refractory compositions, reducing material consumption, introducing waste-free technologies in the production of concrete with increased physical and mechanical characteristics under prolonged exposure to high temperatures on cement binders and waste from the metallurgical industry and reducing environmental pollution. A significant environmental impact on the environment is exerted by large-tonnage technogenic waste produced by JSC «Aluminum of Kazakhstan» – bauxite sludge obtained by processing bauxite into alumina containing 42.7% Fe2O3. The prospects of its application as a filler in heat-resistant concretes are considered, which makes it possible to increase the physico-mechanical and thermal characteristics. The composition and properties of this waste and the change in the properties of heat-resistant concrete during the introduction of filler have been studied. Reactive alumina has been studied, which is 99.9% submicron alumina with a very low content of Na2O oxide. It is shown that the properties of concrete change after the introduction of iron-containing waste in the amount of 5% and reactive alumina – 37.5% and 38.8%. Their volumetric weight, control strength, and other properties are increased. The improvement of physical, mechanical, and thermal characteristics depends on the structure and neoplasms in the obtained samples. Samples of heat-resistant concrete were analyzed using electron probe X-ray spectral qualitative and quantitative microanalysis and X-ray fluorescence spectrometry and it was shown that the iron-alumina waste contributes to the compaction of the structure due to its resistance to delamination and has increased fluidity at low humidity in the cementing mass. For further investigation of the physical-thermal characteristics, depending on the structure and neoplasms in the obtained samples, a petrographic method using a polarization microscope in transmitted and reflected light is required.

Energy Dispersive X-Ray Fluorescence Spectrometry Using a Matrix Corrected Fundamental Parameters Algorithm vs. Acid Digestion with ICP-AES: A Comparison of Two Methods for Soil Elemental Analysis

ABSTRACT Energy dispersive X-ray fluorescence spectrometry (ED-XRF) is evaluated as an alternative to conventional acid-mediated soil digestion methods for analysis of aluminum (Al), calcium (Ca), iron (Fe), potassium (K), magnesium (Mg), manganese (Mn), sodium (Na), phosphorus (P), silicon (Si), strontium (Sr), titanium (Ti), and zirconium (Zr). The Kellogg Soil Survey Laboratory (KSSL) currently uses microwave-assisted digestion with inductively coupled plasma – atomic emission spectrometry (ICP-AES) to measure the 12 elements (Al, Ca, Fe, K, Mg, Mn, Na, P, Si, Sr, Ti, Zr). The equipment needed to conduct the digestion method is expensive, the materials are hazardous, and the method is laborious. The Kellogg Soil Survey Laboratory (KSSL) has observed variable elemental recoveries for certain elements. The objective of the study was to evaluate an ED-XRF method as an alternative to the KSSL digestion method. The literature offers few examples of X-ray fluorescence (XRF) method development and validation. The candidate ED-XRF method offered a more efficient, less expensive, and less hazardous approach for measuring the 12 elements. Relative to the digestion method, the candidate ED-XRF method showed improved precision and accuracy for specific elements.

Simultaneous adsorption of ammonia nitrogen and phosphate on electro-assisted magnesium/aluminum-loaded sludge-based biochar and its utilization as a plant fertilizer.

Herein, Mg/Al-loaded sludge-based biochar was prepared via electro-assisted impregnation. The structure and chemical analysis of modified sludge-based biochar (MgSBC-0.5(@Al) showed that the material was loaded with MgO and Al2O3. The specific surface area of MgSBC-0.5(@Al) was 11.27 times higher than that of unmodified sludge-based biochar (SBC). The simultaneous adsorption performance of MgSBC-0.5(@Al for ammonia nitrogen (NH4+-N) and phosphate phosphorus (PO43--P) was studied. The maximum adsorption capacities of MgSBC-0.5(@Al for NH4+-N and PO43--P at 298 K were 65.19 and 92.10 mg·g-1, respectively, 4.45 and 6.28 times higher than those of SBC. The external and internal elemental compositions of the modified and unmodified biochar specimens were quantitatively characterized using inductively coupled plasma mass spectrometry, X-ray photoelectron spectroscopy, and X-ray fluorescence spectrometry. The results emphasized the importance of Mg-loading for NH4+-N and PO43--P capture. MgO was mainly loaded on the surface of biochar, enabling adsorption through chemical reactions. Analysis showed that the adsorption of NH4+-N and PO43--P on the modified biochar proceeded simultaneously through multiple mechanisms. Particularly, the adsorption of NH4+-N and PO43--P occurred through the precipitation of struvite and physical adsorption, with PO43--P also adsorbed through the formation of MgHPO4 and CaHPO4. Other data indicated that Al, Ca, and Fe had a trapping effect on the adsorbate. Importantly, the biochar after adsorption could be used as a soil amendment.

Unusual Composition of the Sarezzano Reliquary Busts

The interdisciplinary study of two reliquary busts from Sarezzano (Piedmont, Italy) is a perfect example of the necessity to provide for material characterisation as a recurring common practice in historical studies and a mandatory step in conservation assessment. Furthermore, the diagnostics of cultural heritage play a crucial role in art historical research, providing relevant information on artefacts’ genesis, production technology, and conservation history. The study of the materials of the reliquary busts was performed by non-invasive (portable X-ray fluorescence spectrometry) and micro-invasive (stereomicroscope, attenuated total reflection Fourier transform infrared spectroscopy and powder X-ray diffraction analysis) methods. According to the results, the busts were found to be made of a tin–lead alloy, a rather unusual material for mediaeval reliquary busts. Moreover, the outcome suggests that the busts were originally silvered, except for the hair and beard which are still gilded. The analysis reveals the use of colophony as an adhesive buffer layer on the busts’ alloy, as well as inside them, to favour the metal working process, since it is found as degraded residue. Finally, even the typology of alloy decay is defined. All this information has enabled us to determine the artistic technique and estimate the value and quality of the material employed. In addition, it has led to the correct choice of materials and methods to be adopted during the restoration, and therefore the usage of more suitable solvents and tools.

Phase and microstructural characterization of swat soapstone (Mg3Si4O10(OH)2)

Abstract This study focuses on the comprehensive exploration of Swat soapstone, employing a range of analytical techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) spectroscopy, Fourier-transform infrared (FTIR) spectroscopy, and X-ray fluorescence (XRF) spectroscopy. XRD was used to identify the phase and lattice parameters of the soapstone. SEM further scrutinizes the dispersed soapstone particles, revealing different structural characteristics such as a slightly elongated, cubic-like structure, a straight rod-like formation, and a rough, textured surface. EDX spectroscopy was utilized for studying the elemental composition of the soapstone. The analysis identifies talc as the primary mineral in Swat soapstone, with iron, an element, also contributing notably to its composition. This underscores the complexity of Swat soapstone’s internal structure. XRF analysis further contributes to the elemental characterization, revealing a dominant composition of silicon (Si) at 48.567 wt% and a notable contribution from iron (Fe) at 16.108 wt%. FTIR analysis confirmed the absorption of infrared radiation at the non-bridging oxygen (Si–O–) within the silicate network and the Si–O–Si bending vibration. This work investigates the chemical and morphological details of the Swat soapstone.

Ultra-High Adsorption Capacity of Calcium-Iron Layered Double Hydroxides for HEDP Removal through Phase Transition Processes.

Antiscalant disposal in reverse osmosis concentrate (ROC) treatment is a significant obstacle in desalination. This study investigated the adsorption performance of LDHs for removing 1-hydroxyethylidene-1,1-diphosphonic acid (HEDP). CaFe-LDH presented a specific adsorption behavior and ultrahigh adsorption capacity for HEDP, with a maximum adsorption capacity of 335.7 mg P/g (1116.5 mg HEDP/g) at pH 7.0. X-ray diffraction (XRD) demonstrated that HEDP adsorption induced a structural transformation of CaFe-LDH from a layered configuration to a highly ordered structure, leading to a noticeable phase transition. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy further confirmed that two distinct binding modes of HEDP, relating to chelation with Ca2+ and adsorption on Fe3+ simultaneously, are connected by phosphonic acid groups (-C-PO(OH)2), forming the CaFe-HEDP complex. X-ray fluorescence (XRF) and X-ray photoelectron spectroscopy (XPS) analyses revealed that the CaFe-HEDP ternary complex exhibits a highly ordered arrangement in an oxygen-bridged framework. The construction of an oxygen-coordinated framework contributes to the incorporation of more HEDP into CaFe-LDH, leading to a well-aligned lattice in the new phase. These findings provide valuable insights into developing novel LDH-based adsorbents for removing phosphorus-containing antiscalants, establishing a sustainable approach to ROC management, and potential environmental risk reduction.

Zinc determination in common beans by pXRF: An easy and versatile calibration strategy applied to biofortification studies

Zinc deficiency is observed in millions of individuals, especially in underdeveloped countries. Therefore, agronomical strategies have been implemented to mitigate this public health issue, mainly by the biofortification of staple food crops, e.g., common beans, one of the most consumed leguminous grains worldwide. Accurate Zn determination by an analytical method is one of the most relevant steps in these initiatives. This study evaluated three calibration methods for Zn determination by portable X-ray Fluorescence Spectrometry (pXRF) in pelletized common bean samples. A Ti/Al primary filter and a 10-second irradiation time were selected as optimized operating conditions. The sample with the highest Zn content was submitted to acid extraction with diluted HCl and HNO3 to obtain synthetic blanks. Increasing amounts of the original sample were mixed with the obtained blanks to prepare the calibration curves standards. An additional calibration model with plant-based CRMs was also evaluated. Zinc mass fractions calculated using the calibration model of HCl-extracted and mixed samples showed statistical agreement with the reference data as demonstrated by the Student t-test at a 95 % confidence level. The linear correlation factor (r) was greater than 0.99, with a detection limit as low as 2.23 mg kg−1. The obtained calibration model also exhibited high prediction capability, as revealed by the low RMSEP (Root Mean Square Error of Prediction), i.e., 2.16 mg kg−1. We concluded that pXRF is an attractive and cost-effective method for direct, quick, and environmentally friendly Zn determination in common beans.

Origin and distribution of clay minerals in semi-arid Sahelian soils: case of Kori Ouallam watershed, south-western Niger

Abstract This study examines the origin and distribution of clay minerals of the pedological horizons of Kori Ouallam watershed (south-western Niger). It is based on field sampling campaigns and a series of laboratory analyses. A total of 49 samples were analysed, 28 from surface horizons (0–10 cm depth) and 21 from pedological profiles (0–1 m depth). The samples were analysed by X-ray diffraction on bulk and clay (<2 μm) fractions, X-ray fluorescence spectrometry, laser granulometry, organic matter and calcium carbonate content, macroscopic observations (binocular loupe) and scanning electron microscopy equipped with an energy-dispersive spectrometry system. The pedological horizons are characterized by low organic matter contents (<1%) and no calcium carbonate. The particle-size distribution shows net textural differentiation, with a predominance of sandy loam to sandy clay loam textures in the upper horizons and clay loam to clay in the deep horizons. The main major oxides were SiO2 (46.3–89.0%), Al2O3 (5.0–24.2%) and Fe2O3 (1.0–27.9%). Kaolinite (64–98%) is the predominant clay mineral at all horizons, associated with low to moderate proportions of illite (1–34%) and traces of chlorite. Kaolinite is essentially inherited from the parent rock, whereas illite results from chemical alteration by bisialitization of the primary minerals initially rich in potassium feldspar contained in the parent rock. However, soil texture and organic matter vary independently with clay mineralogy. An extended study of all of the pedological facies that make up south-western Niger, combined with supplementary analyses, would further improve our understanding of clay mineralogy in the Sahelian zone.

Evaluation of Some Potentially Toxic Elements and Associated Ecological and Health Risks in Topsoil Samples Adjacent to an Industrial Zone in Turkey.

Potentially toxic element (PTE) pollution as a result of industrial activities remains a global problem that poses serious threats to human and ecological health. PTEs (Al, Fe, Ti, Mn, V, Zn, Cu, Cr, Ni, Pb, Co, and As) are metals or metalloids with biological toxicity. This study analyzed the concentrations of these PTEs and the physicochemical properties of topsoil samples collected from areas near industrial districts in the Samsun province of Turkey to evaluate ecological and health risks, estimating various indexes. The average concentrations of Al, Fe, Ti, Mn, V, Zn, Cu, Cr, Ni, Pb, Co, and As analyzed in 23 topsoil samples by energy-dispersive X-ray fluorescence spectrometry were found as 93,822, 82,410, 6623, 1642, 406, 278, 207, 149, 78, 68, 32, and 10 mg/kg dry weight, respectively. Zn, Cu, Cr, Ni, Pb, and Co levels exceed the maximum contaminant levels in the Turkish Regulation on the Control of Soil Pollution. The average pH values, organic matter, total organic carbon, and nitrogen measured in soil samples were 7.14, 6.11, 0.96, and 0.04%, respectively. The ecological and health evaluation reveals that the studied area is polluted with V, Cu, Zn, As, Ni, and Pb, which may pose a risk to people living in settlements near the industrial district.

Initial evaluation of waste phosphogypsum for its use as a precursor for bioceramic materials

In this study, the phosphogypsum waste taken from various places in the factory dump located in Kėdainiai (Lithuania) was reinspected and characterised by different physico-chemical characterisation methods. The results of X-ray diffraction analysis, thermogravimetric analysis and differential scanning calorimetry, Fourier transform infrared spectroscopy, energy-dispersive X-ray analysis, elemental analysis using inductively coupled plasma optical emission and X-ray fluorescence spectroscopy confirmed that the main crystalline phase of the phosphogypsum waste is gypsum (CaSO4·2H2O). The surface morphology of the investigated materials was analysed using scanning electron microscopy. The specific surface area was determined by the Brunauer–Emmet–Teller method. The pore size distribution of the material produced was obtained using the Barrett–Joyner–Halenda method. This study also demonstrated that the phosphogypsum waste could be successfully used as a precursor for the dissolution-precipitation synthesis of high quality bioceramic calcium hydroxyapatite.

Heterometallic Molecular and Ionic Isomers.

Numerous descriptions of structural isomerism in metal complexes do not list any molecular vs ionic isomers. At the same time, one of the most striking examples of structural isomerism in organic chemistry is molecular urea, which has the same atomic composition as the chemically distinct ionic ammonium cyanate. This iconic organic couple now meets its inorganic heterometallic counterpart. We introduce a new class of structural isomers, molecular vs ionic, that can be consummated in complex and coordinatively unsaturated polynuclear/heterometallic compounds. We report inorganic molecular and ionic isomers of the composition [NaCrFe (acac)3(hfac)3] (acac = acetylacetonate; hfac = hexafluoroacetylacetonate). Heterometallic molecular [CrIII(acac)3-Na-FeII(hfac)3] (1m) and ionic {[CrIII(acac)3-Na-CrIII(acac)3]+[FeII(hfac)3-Na-FeII(hfac)3]-} (1i) isomers have been isolated in pure form and characterized. While both ions are heterobimetallic trinuclear entities, the neutral counterpart is a heterotrimetallic trinuclear molecule. The two isomers exhibit distinctly different characteristics in terms of solubility, volatility, mass spectrometry ionization, and thermal behavior. Unambiguous assignment of the positions and oxidation/spin states of the Periodic Table neighbors, Fe and Cr, in both isomers have been made by a combination of characterization techniques that include synchrotron X-ray resonant diffraction, synchrotron X-ray fluorescence spectroscopy, Mössbauer spectroscopy, and DART mass spectrometry. The transformation between the two isomers that does take place in solutions of noncoordinating solvents has also been tested.

Technological choices and practices of Early Bronze Age pottery production in the Central Plains: Focusing on the sites of Xinzhai and Huadizui

Aspects of the Early Bronze Age (ca. 2050–1640 BCE) pottery production technology and knowledge transfer in the Central Plains of China (i.e., the Zhengzhou-Luoyang area) were studied. To this aim, 120 domestic pottery samples and ten geological samples from two central sites at Xinzhai and Huadizui were studied macroscopically and analysed with X-ray fluorescence spectrometry. Based on a discussion of macroscopical evidence and chemical composition, the results tentatively indicate the technological knowledge transfer between the potters in Xinzhai and Huadizui sites despite being located about 80 km apart. Pottery of the same category was manufactured with similar selection and preparation strategies of ceramic raw materials, decorated with similar patterns, and adopted similar forming techniques. More specifically, the cookware from the Xinzhai and Huadizui sites was hand-made and Ca-poor, while the storage- and drinking wares were wheel-made and Ca-rich. These results likely indicate the existence of one overarching community of practice, potters located at Xinzhai and Huadizui, who shared strategies for raw materials selection, paste preparation, and finishing.

Nondestructive and quick differentiation between loupe-clean low-alkali natural and hydrothermal synthetic aquamarines: Constraints of infrared spectroscopy

A considerable increase in the price of natural aquamarine has led to the emergence of hydrothermal synthetic aquamarine as a cheap substitute in the market. In this study, comparative analysis was conducted between natural aquamarine obtained from Altay Prefecture in Xinjiang, China, and hydrothermal synthetic aquamarine in the Chinese market to distinguish them with loupe-clean clarity. Nondestructive tests including microscopic observation, X-ray fluorescence spectroscopy, infrared spectroscopy, ultraviolet–visible–near-infrared spectroscopy, and Raman spectroscopy were conducted. The two samples were low-alkali aquamarine, dominated by type Ⅰ H2O, and the infrared spectra showed similar water-related peaks, exhibiting weak absorption bands related to Cl− at 2736 and 2449 cm−1 and CO2 in the crystal channels at 2358 cm−1. Apart from the strong irregular and distinctive growth patterns, infrared absorption bands at 3313 and 4060 cm−1 due to the N–H bond (derived from ammonium halide used in crystal growth) vibrations were found to be present only in hydrothermal synthetic aquamarine. This study reveals implications for identifying hydrothermal synthetic aquamarine when the internal features of loupe-clean aquamarine are not obvious.

Particle Conditioning for Improving Blockage Resistance of Denitration Catalysts in Sintering Flue Gas

The stability and safety of selective catalytic reduction (SCR) systems are threatened by potential catalyst blockages caused by fly ash deposition. This paper proposes to improve the blockage resistance of denitration catalysts for sintered fly ash through particle conditioning. X-ray fluorescence spectroscopy, scanning electron microscopy, and laser particle analyzer were combined with laboratory heating experiments and field tests for systematic research. The results indicate that the composition and morphology of sintered fly ash are intrinsic factors contributing to catalyst blockage, while heating conditions act as external triggers. The sintered fly ash primarily exhibits a fluffy, branched cotton-like structure. Its main components are K2O, Fe2O3, Na2O, and CaO, with the alkali metal oxides of potassium and sodium comprising 20% to 50%. At ambient temperature, sintered fly ash presents no agglomeration, but significant agglomeration occurs as temperature increases. Particle conditioning effectively inhibits the agglomeration tendency of sintered fly ash. Field tests show that catalyst activity remains unaffected even under severe blockage conditions. The pressure drop across the catalyst layers increases progressively, with the first layer displaying the least pressure drop and the third displaying the most. After particle conditioning, the pressure drop across the catalyst is stabilized at values below 600 Pa, effectively mitigating the blockage issue in the denitrification catalyst for sintering flue gas. This research provides critical technical support for the stable ultra-low emission of NOx from sintering flue gas.

Study of the structural and phase state of ceramics synthesized from 6YSZ - Al2O3 – HfO2 by semi–dry pressing followed by sintering in vacuum

The study investigates the properties of 6YSZ – Al2O3 – HfO2 powder mixture and the resulting ceramics obtained by semi-dry pressing followed by sintering in vacuum. X-ray fluorescence spectrometry revealed the primary constituents as zirconium (81%), aluminum (8.7%), yttrium (5.7%), and hafnium (3.5%). The average particle diameter was 0.5 μm, with specific surface area and bulk weight recorded at 18,535 cm2/g and 0.84 g/cm3, respectively. X-ray phase analysis indicated a predominance of monoclinic zirconium dioxide. Sintering at 1400-1600°C transformed the phase composition, enhancing density and microhardness, with values peaking at 5.8 g/cm3 and 12.1 GPa at 1600°C. This process also increased the tetragonal phase content to 63%. The ceramics exhibited the highest crack resistance at 1600°C, attributed to the stabilized tetragonal zirconium dioxide. Microstructural analysis confirmed the homogenous distribution of the elements and the presence of fine fractions influencing microstructural properties. 1600°C was found to be the optimal temperature for sintering the 6YSZ – Al2O3 – HfO2 ceramics.

Soil contamination by trace elements and radioelements and related environmental risks in agricultural soils of the M'Dhilla Basin (southwestern Tunisia).

Agricultural soil contaminated by phosphogypsum pile stocked in plan air remains a major problem in M'Dhilla city southwestern of Tunisia. The present effort aimed to enhance the knowledge of trace elements and radioactivity abundance and to assess the corresponding environment. X-ray fluorescence spectroscopy was used to evaluate the trace elements, radioactive elements, and major element concentrations. Our finding revealed that the mean values of U and Th in all the soil profiles ranged from 0.283 to 2.875mg.kg-1 and from 0.797 to 1.491mg.kg-1 respectively. The statistical analyses indicated that uranium abundance has non-significant correlation with the most of trace metals; it shows a moderate correlated with Sr and inverse correlation with P2O5. Contamination factors indicate that the studied soil ranged from uncontaminated to significantly contaminated. Thus, the pollution load index values classify the sites from background values to high pollution sites. The findings of this study will help improve the environmental conditions of M'Dhilla city by addressing contamination issues through targeted interventions. The study's findings highlight the importance of a periodic environmental monitoring such as soil remediation in the study area. This research fills a critical gap in the current understanding of contamination management in this region.

Processing and Characterization of Spent Nickel-Metal Hydride Type AA Batteries to Recover Valuable Materials (Cobalt, Nickel and Rare Earth Elements).

The experimental research was focused on the investigation of valuable material from spent Ni-MH type AA batteries, namely the metal grid anodes and the black mass material (anode and cathode powder). The materials of interest were analyzed by X-ray fluorescence spectroscopy (XRF), ICP-OES (inductively coupled plasma optical emission spectrometry), optical microscopy, scanning electron microscopy (SEM), energy-dispersive X-ray analysis (EDX), electron backscatter diffraction (EBSD), and X-ray diffraction (XRD). The analyzed grids have a high Fe content, but some of them correspond to the Invar alloy with approx. 40% Ni. In the black mass material, round particles and large aggregations were observed by SEM analysis, showing a high degree of degradation. The XRD analysis reveals the presence of only three compounds or phases that crystallize in the hexagonal system: La0.52Ce0.33Pr0.04Nd0.11Co0.6Ni4.4, Ni(OH)2, and La5Ni19. The obtained results provide useful and interesting information that can be used for further research in the recycling and economic assessment of metals from spent Ni-MH batteries.

Palladium-Catalyzed Double Decarboxylative [3 + 2] Annulation of Naphthalic Anhydrides with Internal Alkynes.

A palladium-catalyzed [3 + 2] annulation of naphthalic anhydrides with internal alkynes has been developed. The present protocol offers an efficient and convenient route to access a series of 1,2-disubstituted acenaphthylenes with excellent functional group compatibility. The reaction is proposed to proceed through a double decarboxylation sequence. The reported synthetic protocols can be extended to napthalene- and perylenedicarboximide-containing substrates. The molecular structures, photophysical properties, and frontier molecular orbitals of the obtained adducts were investigated by X-ray crystallography, UV-vis and fluorescence spectroscopy, and DFT calculations.

Effect of primary copper metabolism disturbance on elemental, protein, and lipid composition of the organs in Jackson toxic milk mouse.

Toxic milk (txJ) is an autosomal recessive mutation in the Atp7b gene in the C3H/HeJ strain, observed at The Jackson Laboratory in Maine, USA. TxJ mice exhibit symptoms similar to those of human Wilson's disease (WD). The study aimed to verify organ involvement in a mouse model of WD. TxJ mice and control animals were sacrificed at 2, 4, 8, and 14months of age. Total X-ray Fluorescence Spectroscopy (TXRF) was used to determine the elemental concentration in organs. Tissue chemical composition was measured by Fourier Transform Infrared Spectroscopy (FTIR). Additionally, hybrid mapping of FTIR and microXRF was performed. Elevated concentrations of Cu were observed in the liver, striatum, eye, heart, and duodenum of txJ mice across age groups. In the striatum of the oldest txJ mice, there was lower lipid content and a higher fraction of saturated fats. The secondary structure of striatum proteins was disturbed in txJ mice. In the livers of txJ mice, higher concentrations of saturated fats and disturbances in the secondary structure of proteins were observed. The concentration of neurofilaments was significantly higher in txJ serum. The distribution of Cu deposits in brains was uniform with no prevalence in any anatomic structure in either group, but significant protein structure changes were observed exclusively in the striatum of txJ. In this txJ animal model of WD, pathologic copper accumulation occurs in the duodenum, heart, and eye tissues. Increased copper concentration in the liver and brain results in increased saturated fat content and disturbances in secondary protein structure, leading to hepatic injury and neurodegeneration.