Elemental Analysis Research Articles

New evidence on the Late Bronze – Early Iron Age human nutrition in the Crimea (northern Pontic Region) based on the stable isotope analysis and radiocarbon dating

The application of geochemical methods (stable isotope δ13C, δ15N analysis, chemical elemental analysis and radiocarbon dating) for studying human and animal bones from burials and cultural layers of archaeological sites of Crimea made it possible to highlight the issues of the development of agriculture and cattle-bгeeding during the Late Bronze – Early Iron Ages. One of the controversial questions is the problem of transition from sedentary forms of agriculture and cattle-breeding to mobile cattle-breeding among ancient communities in the Eurasian steppe and forest-steppe. On the base of data obtained various groups of people were identified, which are characterized by different nutritional systems, primarily related to the specifics of their economic activities. The inhabitants of the settlements are characterized by the predominance of fish, seafood, milk and meat. Coastal individuals had access to marine food and C4 plants that they consumed. The presence of various indirect evidence related to land cultivation such as tools for agriculture, suggests the presence of agriculture and the cultivation of millet at the Bai-Kiyat I settlement of the Late Bronze Age by the bearers of the Late Sabatinovka and Early Belozerka cultures. Another group of people from this settlement is associated with pastoral activities. Their diet includes more meat and dairy products, as well as plant foods with photosynthesis of C3. Our research suggests the presence of seminomadic cattle-breeding among the communities of the Sabatinovka and Belozerka cultures of the Late Bronze Age and transhumance pastoralism among the bearers of the Kizil-Koba culture of the Early Iron Age.

Simple and Cost-effective Fabrication of a Supercapacitor Using Carbon Nanoparticle-based Ink

The demand for energy storage devices such as supercapacitors is rapidly increasing in most applications, including electric transportation and portable electronics. The material's high cost and the fabrication complexity of supercapacitors suppress their mass production. In this research, a commercial low-cost conductive ink has been simply painted on flexible stainless steel sheets as supercapacitor electrodes. The ink is mainly based on carbon crystals, as indicated by the X-ray diffraction peaks, and the results of the energy-dispersive X-ray spectroscopy confirm the elemental analysis. The carbon-based ink comprises semi-spherical nanoparticles as imaged by the scanning electron microscope. The electrochemical energy storage mechanism of the carbon nanoparticle-based electrode in the sulfuric acid electrolyte depends on the electric double layer, as investigated by the cyclic voltammetry and the galvanostatic charge-discharge measurements. As a result, the carbon ink-based supercapacitor exhibits a maximum areal capacitance of 0.5 mF/cm2 at 0.25 mA/cm2, a maximum energy of 0.2 µWh, and a maximum power of 1600 µW. The electrochemical impedance spectroscopy shows excellent equivalent series resistance of 0.6 ohm, representing a solid attachment of the ink on the stainless steel substrate. In addition, an angle of 45o in the low-frequency range indicates a semi-infinite diffusion of the electrolyte ions into the nanostructured electrodes. All these elemental, morphological, and electrochemical properties of the carbon-based ink promote its potential to be effortlessly implemented as electrodes, thereby contributing to the advancement of supercapacitor manufacture.

Mass organic matter accumulation induced by rapid redox variations in lakes: Evidence from the Miaoxi area, Bohai Bay Basin, China

The Member 4 of the Paleogene Shahejie Formation (Es4) in the Bohai Bay Basin is interspersed with a set of high-quality source rocks typified as intercalation of red and black mudstones. A large amount of petroleum (crude oil) originates from these source rocks. The Paleocene–Eocene Thermal Maximum (PETM) event occurred during the deposition of Es4 in the Bohai Bay Basin, and the organic matter enrichment model under this event is worth further investigation due to its relationship with and influence on petroleum accumulations. Well LK25-A, as the first oil exploration well drilled into the Es4 in Miaoxi area, serves as a valuable case to study organic matter accumulation. In this study, we integrate total organic carbon (TOC), Rock-Eval pyrolysis, microscopic observation, vitrinite reflectance (VRo), elemental analysis, and gas chromatography–mass spectrometry (GC–MS) to evaluate the hydrocarbon generation potential, organic matter types, thermal maturity, and sedimentary environment of the Es4 in Miaoxi area. The analysis of maceral and rock pyrolysis data reveals that Type I and Type II organic matter make up the majority of Paleogene mudstones in this region. The TOC and rock pyrolysis data show that mudstones in this area have high organic matter abundance and oil-generation potential. The measured vitrinite reflectance distribution of mudstone samples, which ranges from 0.3% to 0.74%, demonstrates that the Paleogene strata are at the immature to mature stage, and the samples from this area contain a sizable amount of bituminite and mineral-bituminous groundmass. The analysis of biomarkers in the mudstone samples indicates that most of the mudstones in this area are in lacustrine and brackish-hypersaline lacustrine environment under a reducing condition, and some of the red mudstones in the Es4 are formed under a suboxic condition. Based on the size and morphology of the pyrite framboid, the redox conditions of the water mass during deposition or diagenesis are further analyzed. The ratio of the size of framboid pyrite (D) to the size of its micrograins (d) suggests that the Es4 black mudstone developed in an anoxic sulfuretted water environment. Both the inorganic and organic geochemical indexes show that the Paleogene paleoclimate has a great influence on the source rocks of Es4 in this area. The distribution of red–black strata in the area is the result of the combined action of the water redox state and the climatic variation during the PETM event. The development models of organic-rich source rocks from the Es3 and Es4 in this area have been created in light of potential connections between rapid redox variation and the PETM event during the Paleogene. These models may offer a theoretical guidance for petroleum exploration in Miaoxi area of Bohai Bay Basin and other contemporaneous continental basins around the world.

A facile approach for fabricating g-C3N4-based materials as metal-free photocatalysts

This study presents a novel, straightforward approach for synthesizing graphitic carbon nitrides (g-C3N4, g-CN) from melamine, requiring merely 30 minutes of thermal holding at temperatures ranging from 400 to 550 °C in an atmosphere comprising either nitrogen or air. Elemental analysis, X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), diffuse reflectance (UV-Vis DRS), photoluminescence (PL) spectroscopy and scanning electron microscopy (SEM) were employed to assess the quality of the as-prepared powders. Furthermore, theoretical calculations utilizing the Density Functional Theory (DFT) method were conducted to reinforce the experimental findings of the research. A further investigation of the thermal stability of the selected sample was conducted using a unique combination of thermogravimetry–coupled with differential scanning calorimetry, quadrupole mass spectrometry (TG-DSC-MS) and advanced temperature-programmed desorption (TPD) analyzes. The current study focuses on the effect of synthesis conditions (temperature and nitrogen/air environment) on the structure, morphology, and photocatalytic performance of g-C3N4 compounds synthesized using this approach. The g-C3N4-based materials were examined as potential photocatalysts using the acid orange 7 (AO7) photodegradation methodology. To enable comparison of the photodegradation experiments, two separate lamps with wavelengths of 360 nm (UV light) and 420 nm (VIS light) were utilized. The primary objective was to present a novel method for the synthesis of g-C3N4-based materials. This was achieved by demonstrating that organic composites generated at lower temperatures have the best photocatalytic capabilities. Furthermore, the approach to achieving high-quality photocatalysts was shown to be cost-effective, environmentally friendly, and scalable.

Use of natural history museum ungulate specimen hair as biomarkers for environmental trace element contamination.

This study reports the first use of natural history museum ungulate specimens' (common fallow deer, bontebok, Arabian oryx, impala, Dall's sheep, water buffalo, and yak) hair as biomarkers for the determination of environmental trace element contamination and public exposure risk factor assessment. Morphological characteristics of the hair, like diameter and protein structure, were determined using optical microscopy and FTIR spectroscopy, respectively. The levels of thirty-nine (39) elements, sixteen (16) rare earth elements (REEs), and selected isotope ratios (52Cr/53Cr, 144Nd/146Nd, 147Sm/149Sm, 173Yb/172Yb, 206Pb/207Pb, and 206Pb/208Pb) in the hair samples were determined by ICP-MS analysis.A NIST 1643e standard reference material was analyzed for method validation to determine the accuracy of the developed elemental analysis method. The average hair diameter found in samples obtained from common fallow deer (193 ± 72µm), bontebok (148 ± 48µm), Arabian oryx (194 ± 40µm), impala (88 ± 20µm), Dall's sheep (240 ± 68µm), water buffalo (139 ± 17µm), and yak (139 ± 16µm) were recorded. 27Al (1642 ± 1551mg·kg-1), 44Ca (506 ± 272mg·kg-1), 56Fe (730 ± 1391mg·kg-1), 24Mg (108 ± 57mg·kg-1), 39K (720 ± 1591mg·kg-1), 28Si (1125 ± 1163mg·kg-1), 23Na (10,223 ± 9824mg·kg-1), and 66Zn (33 ± 25mg·kg-1) have the highest concentrations detected in the hair samples. Potentially toxic elements and REEs have the lowest concentration in the hair samples. The detection of low concentrations of 75As, 111Cd, 59Co, 52Cr, 53Cr, 60Ni, Pb isotopes, and REEs in all hair samples suggests heavy metal contamination. The plausible sources of the detected elements in ungulate animal hair are likely due to dietary intake, anthropogenic activities, environmental contamination, specimens' preservation practices, or a combination of those sources. The figures of merit highlighted by a high correlation coefficient (R2 ≥ 0.9990), low limit of detection (as low as 1.00 × 10-7mg·kg-1 for 140Ce), and high average percent recoveries (97.0 ± 11.5) of the NIST 1643e standard reference material analyses demonstrate the linearity, high sensitivity, and accuracy of the ICP-MS technique for elemental and isotopic analysis of hair samples.

Characterization and Sustainable Applications of Galinsoga parviflora Natural Fibers: A Pathway to Eco-Friendly Material Development

This study investigates the potential of natural fibers extracted from Galinsoga parviflora as sustainable alternatives to synthetic materials, addressing the increasing demand for eco-friendly and biodegradable options in material science. The main objectives were to evaluate the structural, mechanical, and biological properties of these fibers, focusing on their applicability in structural composites. Driven by environmental sustainability, we performed a range of analyses including X-ray Diffraction (XRD) to determine crystallinity and cellulose structure, Fourier-Transform Infrared Spectroscopy (FTIR) to identify functional groups related to biodegradability, and Scanning Electron Microscopy (SEM) to examine surface morphology and fiber dimensions. Key findings include a crystallinity index of 36.3% with cellulose I dominance, a tensile strength of 17.92 MPa, and a modulus of 11.3 GPa, indicating the fibers’ potential for structural applications. Elemental analysis using Energy-Dispersive X-ray Spectroscopy (EDX) revealed a high carbon content (53.0%) and oxygen content (41.3%), along with trace elements that may enhance interaction in polymer matrices. Antibacterial testing demonstrated effective inhibition of Staphylococcus aureus biofilms, with inhibition zones reaching up to 19 mm, comparable to streptomycin. Confocal Laser Scanning Microscopy (CLSM) further confirmed the fibers' biofilm disruption capabilities.Overall, the results highlight that G. parviflora fibers show significant promise as bio-based alternatives for sustainable material development, offering both mechanical strength and biological functionality for future eco-friendly technologies.

Synthesis of Aluminum Complexes Based on 2,6‐Bis(2‐hydroxyphenyl)Pyridines: Efficient Initiators for Ring‐Opening Polymerization of Cyclic Esters

AbstractThe search for new initiators based on nontoxic metal complexes, allowing for the controlled production of polycaprolactone (PCL) and polylactide (PLA) is an actual task. In the present work, we report the synthesis of aluminum complexes 6a and 6b based on substituted 2,6‐bis(2‐hydroxyphenyl)pyridine pro‐ligands. The compositions and structures of the novel compounds were established by elemental analysis and 1H, 13C, NMR spectroscopy in the solid state by X‐ray diffraction analysis (6a and 6b). All the synthesized aluminum complexes are monomeric. Complexes 6a and 6b (in presence of benzyl alcohol (BnOH)) turned out to be active in the ring opening polymerization (ROP) of ε‐caprolactone (ε‐CL), L‐, rac‐lactide (L‐, rac‐LA) gave PCL and PLA with high molecular weights. The mechanism of the polymerization reaction for compounds С, 6a, and 6b was also investigated using the density functional theory (DFT) method. The substituent effect analyzed in terms of percent buried volume and non‐covalent interactions. The values of calculated Gibbs free activation energies correspond to the trend found experimentally.

Comparative Analysis of Calcium Dynamics in Regular-Set Versus Fast-Set Bioceramics: Impact on Cytotoxicity and Apatite Formation.

The objective of this study is to assess the calcium ion (Ca2+) release, pH shift, bioactivity, and cytotoxicity of both forms of EndoSequence Root Repair Material: regular set (ES) and fast set (ESF). ES (n=10) and ESF (n=10) forms were tested for their bioactivity. Elemental analysis was done on the fresh material and material immersed in phosphate buffered saline (PBS) for 30 days. The surface crystal formation was studied. Cytotoxicity was evaluated at different material concentrations using a human hepatocellular cancer cell line (Huh-7). Both materials contain Ca, P, Ta, Zr, and Si as major elements. Both ES and ESF have a limited percentage of Ytterbium and Neodymium. In the fresh material, the ES had a higher Ca2+ concentration with a homogenous surface distribution than ESF. However, ESF released significantly more Ca2+ (p<0.05) and had a higher pH over the 7-day course. When the material was immersed in PBS, the ESF exhibited a significantly higher Ca/P ratio of 2.95, while ES had 2.16 Ca/P ratio (p<0.05). The ESF had a greater capacity to precipitate and grow hydroxyapatite (HA) than ES, resulting in more mature crystals forming on the surface. Both SE and ESF demonstrated low cytotoxicity against Huh-7 cells. When ES and ESF were submerged in simulated bodily fluid, both forms produced apatite crystals at the dentin material interface, releasing high Ca2+ and displaying a prolonged high pH with high bioactivity potential. Both forms had comparable low cytotoxicity. A higher Ca2+ release in ESF indicates dynamic bioactivity, which should be aligned with the clinical requirements.

Synthesis, crystal structures, fluorescence properties, theoretical calculations and substitution effect of mono zinc(II) Schiff base complexes

Six Schiff base zinc(II) complexes were synthesized using 4-methoxyaniline/3-methyl-4-methoxyaniline, aldehydes with different substituents, and zinc chloride by a one-pot method. Their structures were characterized by FT-IR spectra, 1H NMR spectra, elemental analysis (EA), and further by single-crystal X-ray diffraction analysis. The crystal structures of complexes Zn1–Zn5 reveal that the zinc(II) center coordinates with two nitrogen and two chlorine atoms, forming a distorted tetrahedron configuration with geometric indices of 0.87–0.90. However, the central metal adopts a five-coordinate trigonal bipyramidal configuration (τ5 = 0.04) in complex Zn6. Solid-state fluorescence spectroscopy measurements demonstrated that complexes Zn1–Zn6 exhibit the maximum fluorescence emission in the wavelength range of 468–567 nm. Additionally, the substituent groups of the structure can modulate the emission wavelength, which was verified through density functional theory calculations.

Adsorption of malachite green using waste marine cuttlefish bone powder: Experimental and theoretical investigations.

Adsorption remediation is an energy-efficient water treatment technology that utilizes the adsorption properties of a biosorbent to remove various pollutants. While many articles have explored the high surface area and adsorption capacity of activated carbon for remediating aquatic systems, few have delved into the environmental impact of its synthesis, which often involves H3PO4, a highly toxic activating agent. In this study, we present a groundbreaking alternative to activated carbon for the adsorption and remediation of aquatic waste that doesn't rely on chemical products. Our discovery that cuttlefish bone, typically considered waste, can serve as an effective adsorbent is a significant leap in eco-friendly research and a source of inspiration for future sustainable solutions. We selected Malachite Green (MG) as a cationic toxic dye to evaluate the adsorption capacity of our green adsorbent. The prepared powder underwent characterization using techniques such as FTIR, XRD, SEM, and elemental analysis. Additionally, the determination of the cuttlefish bone's zero-point charge pH revealed a value of 8.4, which influences the material's surface charge and its interaction with ions and molecules in the solution. We conducted a detailed study on the effects of solution pH, adsorbent amount, Malachite Green concentration, temperature, and contact time on the dye adsorption. The results demonstrated that the adsorption of Malachite Green by cuttlefish bone powder is an endothermic process, requiring heat input. This indicates that the adsorption efficiency increases with temperature. The significant enthalpy results obtained confirmed the endothermic nature of the process. In this study, we combined experimental and theoretical approaches to gain a better understanding of the adsorption mechanism. The results showed that Cuttlefish Bone is an environmentally friendly and highly efficient adsorbent.

Study on structural alterations and degradation mechanism of lignin from ozone treated scutched flax tow (SFT).

Ozone is commonly used in lignocellulosic fiber extraction and degumming processes because of its selective reactivity with lignin. However, most studies have focused on the removal of non-cellulosic substances from various lignocellulosic fibers (e.g., wood, pulp, bamboo, and sugarcane bagasse) and the conversion and utilization of the obtained lignin. The lignin degradation mechanism in lignocellulosic fibers during ozone degumming/extraction remains poorly understood. In this study, the structural alterations of milled wood lignin (MWL) isolated from scutched flax tow (SFT) before and after ozone treatment were examined using Fourier transform infrared spectroscopy (FTIR), ultraviolet spectroscopy (UV), gel permeation chromatography (GPC), elemental analysis, thermogravimetric analysis (TGA), pyrolysis-gas chromatography-mass spectroscopy (Py-GC/MS) and nuclear magnetic resonance spectroscopy (NMR). The results showed that the MWL from SFT was primarily composed of syringyl (S) and guaiacyl (G) units. 2D HSQC NMR results revealed that the β-O-4' linkages were dominant in the lignin of SFT. After ozone treatment, some of β-O-4' and β-β linkages and most of β-5 linkages were damaged. The S-type units further degraded into G-type units in ozone treatment system. Overall, this work provides a detailed analysis and valuable insights into the delignification mechanism of the widely used ozone degumming/extraction process for lignocellulose fibers.

Design, Synthesis and Pro-Inflammatory Activity of Palmitoylated Derivatives of Thioglycolic Acid as New Immunomodulators.

The immune system is essential for the defense against infections and is critically implicated in various disorders, including immunodeficiency, autoimmunity, inflammation and cancer. The current study includes a new design of palmitoylated derivatives of thioglycolic acids (PTGAs) capable of triggering innate immune responses. The new series were accessible through a three-step synthetic route, including N-palmitoylation, Claisen-Schmidt condensation and thia-Michael addition. Their structures were elucidated using different 1D and 2D NMR spectroscopic techniques and their purity was confirmed by elemental analysis. The most active PTGAs induced a 12-26-fold increase in the expression of TNF-α and IL-1β mRNA and triggered a marked release of NO in isolated macrophages. These levels were comparable to the responses elicited by heat-killed E. coli and S. aureus. The position of the palmitamide chain and aryl substitution had a significant effect on the TNF-α and IL-1β mRNA expression and NO release. Simulations of molecular dockings showed that the new PTGA derivatives occupy the same TLR2/TLR6 heterodimer active binding site of the microbial diacylated lipoproteins. The new immunomodulators may have a profound impact on various clinical disorders associated with dysfunctional innate immunity.

Preparation and properties of a new type of temperature-resistant and salt-resistant fluid loss additive ADIM for oil well cement

In order to adapt to the deep high temperature and high salt cementing operation environment, itaconic acid (IA), N,N-dimethylacrylamide (DMAA), 2-acrylamido-2-methylpropanesulfonic acid (AMPS) and heterocyclic alkenes (R) were used as polymerization monomers in this paper. A temperature-resistant and salt-resistant fluid loss additive named ADIM was successfully prepared by free radical aqueous solution polymerization and orthogonal experiment. Thermogravimetric, infrared, nuclear magnetic resonance, and elemental analysis have been utilized for assessing the copolymers' structure and heat resistance. The results showed that the target copolymers with thermal decomposition temperature up to 300 ℃ were successfully prepared. A methodical evaluation was conducted on ADIM's application performance. The results show that when the ADIM content is 5 %, the water loss of fresh water cement slurry is only 44 mL at 220 ℃, and the water loss of saturated brine cement slurry is only 64 mL at 180 ℃.In addition to the excellent temperature resistance and salt resistance, the overall performance of ADIM is also good. The mechanism of ADIM was studied by mercury intrusion experiment, scanning electron microscope and TOC test. The results show that ADIM can be adsorbed on the cement particles, effectively reducing the porosity and pore size of the filter cake, thereby reducing the water loss of the cement slurry. ADIM has excellent temperature and salt resistance, which is of great significance for guiding the development of deep oil and gas resources.

Synthesis, DPPH Radical Scavenging, Cytotoxic Activity, and Apoptosis Induction Efficacy of Novel Thiazoles and Bis-thiazoles.

Heterocyclic materials-containing thiazoles exhibited incredible importance in pharmaceutical chemistry and drug design due to their extensive biological properties. Synthesis of thiazoles and bis-thiazoles from the reaction of 2-((6-Nitrobenzo[ d][1,3]dioxol-5-yl)methylene)hydrazine-1-carbothioamide with hydrazonoyl chlorides in dioxane and in the existence of triethylamine as basic catalyst. The antioxidant, in vitro antiproliferative, and cytotoxicity efficacy of thiazoles and bis-thiazoles were measured. In this work, novel series of 5-methyl-2-(2-(-(6-nitrobenzo[d][1,3]dioxol-5-yl)methylene) hydrazinyl)-4-(aryldiazenyl)thiazoles (4a-f) were prepared via the reaction of hydrazonoyl chlorides 2a-f with 2-((6-nitrobenzo[d][1,3]dioxol-5-yl)methylene)hydrazine-1-carbothioamide (1) in dioxane and employing triethylamine as basic catalyst. Following the same procedure, bisthiazoles (6, 8, and 10) have been synthesized by utilizing bis-hydrazonoyl chlorides (5, 7, and 9) and carbothioamide 1 in a molar ratio (1:2), respectively. The distinctive features in the structure of isolated products were elucidated by spectroscopic tools and elemental analyses. The antioxidant, in vitro anti-proliferative, cytotoxicity, and anti-cancer efficacy of thiazoles and bis-thiazoles were evaluated. Compounds 4d and 4f were the most potent antioxidant agents. Gene expression of apoptosis markers and fragmentation assay of DNA were assessed to explore the biochemical mechanism of synthesized products. Thiazoles significantly inhibited cell growth and proliferation more than bis-thiazoles. They induced apoptosis through induction of apoptotic gene expression P53 and downregulation of antiapoptotic gene expression Bcl-2. Moreover, they induced fragmentation of DNA in cancer cells, indicating that they could be employed as anticancer agents by inhibiting tumor growth and progression and can be considered effective compounds in the strategy of anti-cancer agents' discovery. Synthesis, DPPH Radical Scavenging, Cytotoxic activity, and Apoptosis Induction Efficacy based on Novel Thiazoles and Bis-thiazoles.

Organogermanium(IV) complexes with O,N,O’-tridentate Schiff bases: synthesis, electrochemical transformations, photophysical properties, and anti/prooxidant activity

A series of novel diorganogermanium(IV) complexes of the type [R2Ge(Ln)] (where R is Et, Ph) with O,N,O’-tridentate redox-active Schiff bases has been synthesized. Compounds 1–7 were characterized by 1H, 13C{1H} NMR, IR spectroscopy, and elemental analysis. The molecular structures of complexes 1, 3, and 7 in crystal state have been established using single-crystal X-ray analysis. The complexes are pentacoordinate mononuclear compounds of germanium(IV). The bond lengths in tridentate ligands correspond to their diamagnetic dianionic forms. The electrochemical properties of complexes 1–7 were studied by cyclic voltammetry. A feature of the electrochemical behavior of target complexes is the ability to form relatively stable reduced/oxidized species as a result of the one-electron transfer. The stability of electrogenerated forms is influenced by both the organic groups at the germanium(IV) atom and the substituents in the Schiff bases. The energy gap (ΔEel) between the boundary redox orbitals obtained from electrochemical data for the complexes varies from 2.43 to 2.60 eV, while the optical ΔE was observed in the narrow range (2.46 – 2.50 eV). Luminescent activity was detected for some complexes in the solution. The maximal values ​​of the relative quantum yield were determined for complexes containing an electron-withdrawing nitro group in the redox-active ligand. In the reaction with ABTS radical cation, compound 1 only possessed the radical scavenging activity while the other compounds are characterized by weak neutralizing properties. The dual anti/prooxidant action was observed for compounds 1–7 in the process of rat liver (Wistar) homogenate lipid peroxidation.

Mineralogical Characteristics and Purification Experiments of Quartz from a Pegmatite: A Case Study in the Lushi Region of the Qinling Orogenic Belt, Central China

This study uses a sample of pegmatite (LS-1) from the Longquanping deposit in Lushi County, Henan Province, to evaluate its potential as a valuable source of HPQ. This investigation uses various analytical techniques to assess the quality of quartz and its suitability for industrial applications. The methods used in this study include optical microscopy, scanning electron microscopy (SEM), Raman spectroscopy, X-ray fluorescence spectrometry (XRF), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), and inductively coupled plasma mass spectrometry (ICP-MS) to analyze the petrographic, mineralogical, and trace element characteristics of quartz before and after purification and comprehensively evaluate the potential of quartz in these rocks as an HPQ raw material ore. The optical and scanning electron microscopic observations reveal several impurities and associated minerals in quartz, including feldspar, biotite, magnetite, sphene, and large number of fluid inclusions composed of both gas and liquid phases. The content of trace element in raw quartz ore in the LS-1 sample as determined by LA-ICP-MS analysis ranges from 41.61 to 256.13 ppm, with the main impurity elements being Al, Ti, Li, Na, K, and Ca. After purification, the SiO2 contents and total trace elements contents of the LS-1 refined quartz sand was 99.997 wt.% and 29.29 ppm, respectively, with Al (13.29 ppm), Ti (4.20 ppm), Li (1.15 ppm), and Na (10.32 ppm). The major trace element contents of Al and Ti in the quartz concentrates were lower than the upper limit of the HPQ standard and thus belonged to the high-end products (4N8). Results of this study show that quartz from a pegmatite in the Lushi region has the potential to be purified HPQ. This study underscores the importance of thorough mineralogical and elemental analyses in assessing the suitability of quartz raw material deposits for HPQ production.

Nickel (II) and Copper (II) Schiff Base Derivatives: Design, Characterization, Biological Activity

AbstractThis work presents the designing and characterization of two novel metal complexes derived from a Schiff base, N,N’‐ethane‐1,2‐diylbis[1‐(2‐chloroquinolin‐3‐yl)methanimine] (EBCQ), coordinated with Ni (II) (NiEBCQ), and Cu (II) (CuEBCQ). Structures of the metal complex derivatives were proposed utilizing a variety of analytical methods having elemental analysis, ultraviolet‐visible spectroscopy, mass spectroscopy, infrared spectroscopy, magnetic properties, conductivity measurement, and thermal analysis. The obtained data revealed octahedral geometries for both NiEBCQ and CuEBCQ complexes, denoted as [Ni(EBCQ)(H2O)2(Cl)2] and [Cu(EBCQ)(H2O)2(Cl)2], respectively. Density functional theory computations were employed for confirming the molecular structures and exploring quantum chemical parameters of both EBCQ and its metal complex derivatives. The anti‐inflammatory results reveal that the EBCQ ligand and its metal complexes, NiEBCQ, and CuEBCQ, exhibit varying degrees of inhibition, with CuEBCQ showing the highest potency. CuEBCQ achieved 89.80% inhibition at 300 µM, with an IC50 value of 86.38 µM, indicating its superior anti‐inflammatory activity compared to NiEBCQ (IC50 of 92.33 µM) and the ligand EBCQ (IC50 of 169.07 µM). In the antioxidant assays, the CuEBCQ complex again showed the most pronounced activity, achieving an IC50 of 74.16 µM, outperforming both NiEBCQ (IC50 of 89.06 µM) and the EBCQ ligand (IC50 of 101.58 µM). The antibacterial tests confirmed the metal complexes' superiority, particularly CuEBCQ, which displayed excellent inhibition against Bacillus cereus compared to the ligand. Molecular docking studies targeting specific proteins (5IKT for human cyclo‐oxygenase‐2, and 5IJT for human peroxiredoxin 2) were performed to assess the binding affinities and interactions of EBCQ and its metal complex derivatives. The results propose promising potential for the application of EBCQ and its metal complexes as novel therapeutic agents with diverse biological activities. Finally, antibacterial effectiveness of the ligand and its complexes were monitored opposed to several Gram‐positive and Gram‐negative bacteria.

Mathematical calculation of the boundary conditions for zinc sulfide-selenide formation in the hydroxide-hydrazine-thiourea-selenium system

Based on thermodynamic constants, the concentration limits of the initial zinc-containing salt and the range of pH values at which the depositions of ZnS and ZnSe without Zn(OH)2 are possible were calculated. The boundary conditions of the formation of the ZnSxSe1–x solid solution in the hydroxide-hydrazine-thiourea-selenium system were defined by the overlap area between the constructed ZnS and ZnSe formation zones. The task of complex intermolecular interaction between complexed zinc ions and two chalcogenizers in the working solution was solved on the basis of mathematical calculations. A sample of the ZnSxSe1–x film was deposited within the calculated area of its formation, which was confirmed by X-ray diffraction and elemental analysis.

Preparation, Structural Identification, and Biomedical Evaluation of Some New Complexes

A new nano azo ligand, [2-amino-6-oxo-6,7-dihydro-1H-purin-8-yl)diazenyl)nitrobenzene (AH), and its Ag(I), Cu(II), and Zn(II) complexes were successfully synthesized and characterized using elemental analyses, magnetic susceptibility, molar conductance, and spectroscopic techniques (FTIR, UV-vis, ¹H-NMR), along with thermal analysis. FTIR confirmed the ligand acts as a neutral N,N-bidentate. The metal-to-ligand ratio was determined to be 1:1 for Ag(I) and Zn(II) complexes and 1:2 for the Cu(II) complex. Stability constants and Gibbs free energy, assessed via spectrophotometry, indicated high stability for all complexes. SEM and X-ray diffraction revealed nanoscopic properties for the Ag(I) and Cu(II) complexes. The antimicrobial activity against Staphylococcus aureus, Klebsiella pneumoniae, and Candida albicans species showed good efficiency compared to reference drugs. The ligand also exhibited moderate antioxidant activity using the DPPH assay. Additionally, the Zn(II) complex demonstrated effective anti-inflammatory activity, promoting wound healing within 14 days, compared to 16 days with silver sulfadiazine and 18 days without treatment.

In vitro studies of the combination between berberine chloride and a Copper(II) complex against Triple negative breast cancer

In this study, the copper(II) complex [Cu(chromoneTSC)Cl2]•0·.5H2O•0.0625C2H5OH (where chromoneTSC = (E)-N-Ethyl-2-((4-oxo-4H-chromen-3-yl)methylene)-hydrazinecarbothioamide) was synthesized and characterized; then used to carry out in vitro studies in combination with berberine chloride (BBC). The ligand and complex were characterized by elemental analysis, FTIR and NMR (1H and 13C) spectroscopy, and conductivity measurements. The cytotoxic effect was analyzed by using the CCK-8 viability assay in cancer MDA-MB-231 VIM RFP and non-cancer MCF-10A cell lines. The IC50 values for the complex and BBC were 21.2 ± 1.6 and 48.3 ± 2.4 μM, respectively at 24 h incubation, while the IC50 value of the combination treatment was 9.3 ± 1.5 in cancer cells. The co-treatment group significantly increased the number of cells in G2 phase, indicating the growth arrest of cancer cells. Moreover, the combination group showed induction of both intrinsic and extrinsic apoptotic pathways. There was also a study on the effect of the combination treatment on receptor-interacting serine/threonine-protein kinase 3 (RIPK3) and mixed lineage kinase domain-like pseudokinase (MLKL) as biomarkers of necroptosis. The results showed activation of necroptosis after treatment with the combination of the copper complex and BBC via the activation of RIPK3–MLKL pathway.