ICP-AES Research Articles

Use of <i>Hermetia illucens</i> hermicompost in the technology of growing legume microgreens

Relevance. The work describes the prospect of using black soldier fly zoohumus as an organic fertilizer to activate the growth of microgreens of non-traditional legume species, including small-seeded ones, and the prospects of reducing the dose of mineral fertilizers.Methods. An experiment was carried out with a comparative study of changes in the morphometric and chemical parameters of plant growth at the full recommended dose of mineral fertilizers, and at 25% of their use, but with the addition of 1% liquid extract of zoohumus, also enriched with essential elements. The duration of the experiment was 21 days. The plants were grown in a closed grow tent, with intensive light culture and control of the internal microclimate of the working area.Results. Among the six studied non-traditional legume species grown for microgreens, the most responsive to combined treatment with an organomineral complex was Onobrychis viciifolia. Trifolium rubens showed the worst result in terms of biomass. Analysis of changes in the profile distribution of essential elements in the resulting green biomass, carried out using inductively coupled plasma atomic emission spectroscopy (ICP-AES), revealed iron and zinc ions as potential targets associated with yield shortfalls in juvenile shoots. Since in global food systems these microelements are the most common nutrients noted for the manifestation of “hidden hunger”, especially among children under 5 years of age and women of childbearing age, when creating a nutritional biocomposition based on black soldier fly zoohumus for growing non-traditional types of legumes, further the emphasis should be on them. No significant differences were found in the number of macroelements.Results. The results of the study confirmed the high efficiency of using humic fertilizers in conditions of low soil fertility and revealed the selective sensitivity of vegetable crops to humic preparations of various origins.

Geochemistry and the optics of geospatial analysis as a preposition of water quality on a macroscale.

The water treatment depends exclusively on the identification of residues containing toxic chemical elements accumulated in NPs (nanoparticles), and ultrafine particles sourced from waste piles located at old, abandoned sulfuric acid factories containing phosphogypsum requires global attention. The general objective of this study is to quantify and analyze the hazardous chemical elements present in the leachate of waste from deactivated sulfuric acid factories, coupled in NPs and ultrafine particles, in the port region of the city of Imbituba, Santa Catarina, Brazil. Samples were collected in 2020, 2021, and 2022. Corresponding images from the Sentinel-3B OLCI satellite, taken in the same general vicinity, detected the levels of absorption coefficient of Detritus and Gelbstoff (ADG443_NN) in 443m-1, chlorophyll-a (CHL_NN (m-3)), and total suspended matter (TSM_NN (g m-3) at 72 points on the marine coast of the port region. The results of inductively coupled plasma atomic-emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) demonstrate that the leaching occurring in waste piles at the port area of Imbituba was the likely source of hazardous chemical elements (e.g., Mg, Sr, Nd, and Pr) in the environment. These leachates were formed due to the presence of coal pyrite and Fe-acid sulfates in said waste piles. The mobility of hazardous chemical elements potentiates changes in the marine ecosystem, in relation to ADG443_NN (m-1), CHL_NN (m-3), and TSM NN (g m-3), with values greater than 20gm-3 found in 2021 and 2022. This indicated changes in the natural conditions of the marine ecosystem up to 30km from the coast in the Atlantic Ocean, justifying public initiatives for water treatment on a global scale.

Relationship between ceramic additives and improved biodegradability, osseointegration, and surface roughness of Ni–Ti shape memory alloy for use in load-bearing bone site applications

To make metallic biomaterial implants acceptable for use in bone replacement applications, this research aimed to identify a potential means of improving the poor wear resistance of implants as well as their limited osseointegration capability and rapid biodegradation. In this regard, mechanical alloying was used to make a nickel-titanium (Ni–Ti) shape memory alloy with increasing amounts of hardystonite (HT) and niobium carbide (NbC). X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to examine the phase composition and microstructure of the sintered samples. To test osseointegration and biodegradation, samples were immersed in simulated body fluid (SBF). They were then analyzed using SEM, weight loss measurements, and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The SEM pictures indicated that increasing HT and NbC helped build apatite layers on their surfaces, anticipating successful osseointegration if utilized as bone implants. ICP findings showed that HT and NbC significantly reduced Ni2+ ion release, preventing tissue damage. In contrast to electrical conductivity, these ceramics improved the compressive strength and microhardness of the examined samples. The improvement in their strength was 10.81, 27.02, 21.62, and 31.89 %. SEM results confirmed the role of ceramic materials to enhance the wear resistance of the tested samples. Based on these findings, the prepared nanocomposites achieved the main goal of this study.

On-Line pH Measurement Cation Exchange Kinetics of Y3+-Exchanged Alginic Acid for Y2O3 Nanoparticles Synthesis.

A new sol-gel method that employs cation exchange from an aqueous metal ion solution with H+ ions of granulated alginic acid was developed for synthesizing high-purity Y2O3 nanoparticles. In this study, the cation exchange kinetics of H+~Y3+ in aqueous solution were analyzed using on-line pH technology and off-line inductively coupled plasma-atomic emission spectrometry (ICP-AES) analysis. Pseudo 2nd-order models were utilized to evaluate the parameters of the kinetics, suggesting that the concentration of H+~Y3+ involved in the cation exchange reaction was 1:1.733. Further, a comprehensive understanding of the Y-ALG calcination process was developed using thermo-gravimetric analysis, along with results obtained from differential scanning calorimetry (TGA/DSC). A detailed analysis of the XRD Rietveld refinement plots revealed that the crystallite sizes of Y2O3 nanoparticles were about 4 nm (500 °C) and 15 nm (800 °C), respectively. Differential pulse voltammetry (DPV) was employed to investigate the electrochemical oxidation of catechol. The oxidation peak currents of catechol at Y2O3 (500 °C)/GCE and Y2O3 (800 °C)/GCE showed two stages linear function of concentration (2.0~20.0 × 10-6 mol/L, 20.0~60.0 × 10-6 mol/L). The results indicated that the detection limits were equal to 2.4 × 10-7 mol/L (Y2O3 (500 °C)/GCE) and 7.8 × 10-7 mol/L (Y2O3 (800 °C)/GCE). The study not only provided a method to synthesize metal oxide, but also proposed a promising on-line pH model to study cation exchange kinetics.

Physico-Chemical Properties of CdTe/Glutathione Quantum Dots Obtained by Microwave Irradiation for Use in Monoclonal Antibody and Biomarker Testing.

In this report, we present the results on the physicochemical characterization of cadmium telluride quantum dots (QDs) stabilized with glutathione and prepared by optimizing the synthesis conditions. An excellent control of emissions and the composition of the nanocrystal surface for its potential application in monoclonal antibody and biomarker testing was achieved. Two samples (QDYellow, QDOrange, corresponding to their emission colors) were analyzed by dynamic light scattering (DLS), and their hydrodynamic sizes were 6.7 nm and 19.4 nm, respectively. Optical characterization by UV-vis absorbance spectroscopy showed excitonic peaks at 517 nm and 554 nm. Photoluminescence spectroscopy indicated that the samples have a maximum intensity emission at 570 and 606 nm, respectively, within the visible range from yellow to orange. Infrared spectroscopy showed vibrational modes corresponding to the functional groups OH-C-H, C-N, C=C, C-O, C-OH, and COOH, which allows for the formation of functionalized QDs for the manufacture of biomarkers. In addition, the hydrodynamic radius, zeta potential, and approximate molecular weight were determined by dynamic light scattering (DLS), electrophoretic light scattering (ELS), and static light scattering (SLS) techniques. Size dispersion and the structure of nanoparticles was obtained by Transmission Electron Microscopy (TEM) and by X-ray diffraction. In the same way, we calculated the concentration of Cd2+ ions expressed in mg/L by using the Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-OES). In addition to the characterization of the nanoparticles, the labeling of murine myeloid cells was carried out with both samples of quantum dots, where it was demonstrated that quantum dots can diffuse into these cells and connect mostly with the cell nucleus.

Analysis of Zinc and Copper Content in Selected Tissues and Organs of Wild Mallard Ducks (Anas platyrhynchos L.) in Poland.

The research material included selected muscles and liver of mallard ducks obtained in two research areas. A total of 28 mallards were obtained for the study-six males and six females from the Siedlce hunting district and eight males and eight females from the Leszno hunting district. Zinc and copper concentrations were determined by inductively coupled plasma optical emission spectrometry (ICP OES). It was concluded from the study that the Leszno hunting district is more polluted than the Siedlce hunting district. Among the examined tissues of mallard ducks from both hunting districts, the highest content of zinc and copper was found in the liver. In this organ, birds shot in the Leszno hunting district were characterized by a significantly higher content of these elements compared to birds shot in the Siedlce hunting area. The significantly higher average zinc and copper concentrations in the liver of mallards harvested in this hunting district may have been influenced by fertilization of crop fields in this area with fertilizers containing these elements and by extraction of ore containing zinc and copper minerals in the Legnica-Głogów Copper District. This is an important problem with regard to the safety of consumers of game meat. It was shown that the tissues of male mallards were characterized by higher average levels of zinc and copper than those of females, but the differences were statistically significant only in the case of the average copper content in the leg muscles.

Characteristics and health implications of fine particulate matter near urban road site in Islamabad, Pakistan

The escalating issue of air pollution has become a significant concern in urban regions, including Islamabad, Pakistan, due to the rise in air pollutant emissions driven by economic and industrial expansion. To gain a deeper understanding of air pollution, a study was conducted during winter 2022–2023, assessing physical, chemical, and biological factors in Islamabad. The findings revealed that the average concentration of fine particulate matter (PM2.5) was notably greater than the World Health Organization (WHO) guidelines, reaching 133.39 μg/m³. Additionally, the average concentration of bacteria (308.64 CFU/m³) was notably greater than that of fungi (203.55 CFU/m³) throughout the study. Analytical analyses, including SEM-EDS and FTIR, showed that the PM2.5 in Islamabad is composed of various particles such as soot aggregates, coal fly ash, minerals, bio-particles, and some unidentified particles. EF analysis distinguished PM2.5 sources, enhancing understanding of pollutants origin, whereas Spearman's correlation analysis elucidated constituent interactions, further explaining air quality impact. The results from the Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-OES) indicated a gradual increase in the total elemental composition of PM2.5 from autumn to winter, maintaining high levels throughout the winter season. Furthermore, a significant variation was found in the mass concentration of PM2.5 when comparing samples collected in the morning and evening. The study also identified the presence of semi-volatile organic compounds (SVOCs) in PM2.5 samples, including polycyclic aromatic hydrocarbons (PAHs) and phenolic compounds, with notable variations in their concentrations. Utilizing health risk assessment models developed by the US EPA, we estimated the potential health risks associated with PM2.5 exposure, highlighting the urgency of addressing air quality issues. These findings provide valuable insights into the sources and composition of PM2.5 in Islamabad, contributing to a comprehensive understanding of air quality and its potential environmental and health implications.

Tunning of catalytic performance in coupling, reduction and oxidation of hydrothermal assisted mixed metal oxides of Pd and Cu loaded over mesoporous nanostructure titania coated N‐doped silica using rice husk

Silica–titania‐based mesoporous nanomaterials due to their widespread availability and inexpensive cost have been employed in an extensive range of applications, including heterogeneous catalysis. This research article discusses the hydrothermal synthesis of highly efficient heterogeneous nanocatalyst, that is, mixed metal oxides of Pd and Cu immobilized over silica–titania mesoporous nanostructure and its application in coupling, reduction and oxidation reactions. It was characterized by Fourier transform infrared spectroscopy (FTIR), powder X‐ray diffraction (P‐XRD), field emission gun–scanning electron microscopy (FEG‐SEM), energy‐dispersive X‐ray analysis (EDX), high‐resolution transmission electron microscopy (HR‐TEM), X‐ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), UV–visible spectroscopy (UV–VIS), Brunauer–Emmett–Teller (BET), X‐ray resonance fluorescence (XRF), photoluminescence (PL) and inductively coupled plasma–atomic emission spectroscopy (ICP‐AES) studies to assemble information regarding various structural features. XPS analysis successfully confirmed the presence of mixed oxidation state of Pd and Cu, that is, Pd(0), Pd(II), Cu(0), Cu(I) and Cu(II) over the nanocatalytic support. TEM images showed that the PdCu alloy had spherical shape with average size between 3 and 4 nm. BET analysis indicated that the catalyst has specific surface area of 57.296 m2 g−1 with average pore diameter of 1.84 nm. The results of TGA and DTA analysis demonstrated that the maximum temperature up to which PC‐TNS can catalysed organic reactions was 170°C. The average crystallite size of PC‐TNS was came around 16.08 nm calculated using Scherrer's equation. Moreover, synthesized heterogeneous nanocatalyst was highly recyclable and FEG‐SEM, P‐XRD and XPS findings confirmed the structural disruption after sixth or seventh catalytic run resulted in decrease in yield of products. In general, nanocatalysts can be convincingly more superior to other heterogeneous nanocatalyst due to their unique features such as high specific surface area, high reusability, high reactivity, high product yield and environmentally friendly.

Assessment of potentially toxic and mineral elements in paddy soils and their uptake by rice (Oryza sativa L.) with associated health hazards in district Malakand, Pakistan

Rice, a primary food source in many countries of the world accumulate potentially harmful elements which pose a significant health hazard to consumers. The current study aimed to evaluate potentially toxic and mineral elements in both paddy soils and rice grains associated with allied health risks in Malakand, Pakistan. Rice plants with intact root soil were randomly collected from paddy fields and analyzed for mineral and potentially toxic elements (PTEs) through inductively coupled plasma optical emission spectrometry (ICP‒OES). Through deterministic and probabilistic risk assessment models, the daily intake of PTEs with allied health risks from consumption of rice were estimated for children and adults. The results of soil pH (< 8.5) and electrical conductivity (EC > 400 μs/cm), indicated slightly saline nature. The mean phosphorus concentration of 291.50 (mg/kg) in soil samples exceeded FAO/WHO permissible limits. The normalized variation matrix of soil pH with respect to Ni (0.05), Ca (0.05), EC (0.08), and Mg (0.09), indicated significant influence of pH on PTEs mobility. In rice grains, the mean concentrations (mg/kg) of Mg (463.81), Al (70.40), As (1.23), Cr (12.53), Cu (36.07), Fe (144.32), Mn (13.89), and Ni (1.60) exceeded FAO/WHO safety limits. The transfer factor >1 for K, Cu, P and Zn indicated bioavailability and transfer of these elements from soil to rice grains. Monte Carlo simulations of hazard index >1 for Cr, Zn, As, and Cu with certainties of 89.93% and 90.17%, indicated significant noncarcinogenic risks for children and adults from rice consumption. The total carcinogenic risk (TCR) for adults and children exceeded the USEPA acceptable limits of 1×10−6 to 1×10−4, respectively. The sensitivity analysis showed that the ingestion rate was a key risk factor. Arsenic (As) primarily influenced total cancer risk (TCR) in children, while chromium (Cr) significantly impacted adults. Deterministic cancer risk values slightly exceeded probabilistic values due to inherent uncertainties in deterministic analysis. Rice consumption poses health risks, mainly from exposure to Cr, Ni and As in the investigated area.

Nutritional profile and risk assessment of inorganic elements in enteral and parenteral nutrition formulas

The contents of essential (Ca, Fe, K, Na, P, and Zn) and potentially toxic inorganic elements (As, Al, Cd, Cr, Cu, Mn, and Pb) in enteral and parenteral nutrition formulas were evaluated by inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GFAAS). A total of 30 enteral formulas, 23 parenteral solution components, and 3 parenteral solutions were analyzed. The elements Ca and K presented the higher contents (72–2918 mg L−1 and 235–2760 mg L−1) while the lowest concentration levels were found for As and Cd (<0.68 µg L−1 and <0.01–0.62 µg L−1) in the studied samples. The validated analytical methods presented an accuracy of 75–116% and RSD values lower than 9.8%. Calcium gluconate and magnesium sulfate, which are used as raw materials in parenteral solution, are potential sources of Al and Mn contamination. A Hazard Quotient (HQ) >1 was obtained for Al (27 ± 1 µg L−1) in one of the parenteral samples, whereas the established limit is 25 µg L−1. Enteral samples were considered safe for consumption regarding the Al, As, and Cd levels. One healing-specific and pediatric formula contained Pb at levels above 0.25 µg kg-day−1, too high for safe consumption. The enteral formulas (pediatric, diabetes-specific, renal-specific, healing-specific, and standard formula with addition of fiber) presented risks in relation to the consumption of Cr and Mn (>250 µg day−1 and >11 mg day−1). The results indicate the need for strict monitoring, considering that these formulations are often the single patient’s food source.

Assessment of essential and potentially toxic metals in raw cow milk from Mukaturi town, Oromia Regional State, Ethiopia

Cow milk is a complete and highly nutritious source of food for humans. However, the quality of milk products has become a significant health concern for consumers, particularly infants and children, in many developing nations, including Ethiopia. The objective of this study was to determine the heavy metal levels in raw cow milk collected from dairy producers and collection centers in Mukaturi town, Ethiopia. Sixty raw cow milk samples (40.0 milk samples from dairy farms and 20.0 milk samples from collection centers) were randomly collected and digested using a mixture of nitric acid (HNO3), hydrogen peroxide (H2O2) and perchloric acid (HClO4) on a hot plate. The amounts of heavy metals (Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Zn) in the milk samples were determined using inductively coupled plasma atomic emission spectroscopy (ICP–OES). The findings showed that the average concentrations of Pb (2.31 ± 0.127), Fe (0.566 ± 0.130), Ni (0.210 ± 0.0189), Cd (0.0372 ± 0.0230), Cr (0.369 ± 0.0162), and Co (0.225 ± 0.0150) in mgL−1 were higher than the allowable limits. This could pose a health risk to the public. However, the concentrations of Mn (0.044 ± 0.0369), Cu (0.195 ± 0.0450) and Zn (2.90 ± 0.0570) in mg L−1 were lower than or within the recommended limits and cannot pose any threat to consumers. The validity of the digestion processes was checked by the recovery test. The percentage recoveries of Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Zn were found to be in the range of 80.7–122 %, which is within the acceptable range. Therefore, special attention should be given to the continuous monitoring of heavy metal levels in raw milk among dairy producers and collection centers to minimize economic losses and the risk to consumer safety.

Synthesis and characterization of luminescent cerium-doped hydroxyapatite

Hydroxyapatite (HAp) biomaterials are intended for use as bone substitutes, target functional agents in theranostics or bioimaging due to affinity for hard tissues, biocompatibility, and bioactivity. This study is devoted to HAp doped with cerium, having distinctive feature to change the oxidation state (3+/4+), which affects the physico-chemical and optical properties of the obtained powders. Cerium-doped HAp nanopowders with Ce content up to 0.5 wt% were obtained through precipitation technique and then were heat treated. The following conditions for heat treating were used: (i) heating in air atmosphere, (ii) hot pressing, (iii) heating in a carbon filling. For characterization, the complex methodology was implemented, including X-ray diffraction (XRD) analysis and high temperature XRD, X-ray absorption near edge structure (XANES) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, inductively coupled plasma atomic emission spectrometry (ICP-AES), transmission electron microscopy (TEM), electron paramagnetic resonance (EPR) spectroscopy, and, finally, photoluminescence (PL) spectroscopy. It was shown that the monophase cerium-HAp is stable up to a temperature of 1000 °C in the oxidizing atmosphere, above 1000 °C cerium(4+) oxide forms. Using reducing atmosphere during heating prevents the transition of Ce3+ to Ce4+. PL, EPR and XANES studding clarified obviously the Ce3+ content in the materials obtained under different processing conditions. It was shown, that Ce-HAp powders produced by precipitation and hot pressing contain Ce3+ and exhibit luminescence. The significant luminescence of hot pressed Ce-HAps was caused by a higher concentration of Ce3+ ions and incorporation of carbonate ions as a result of the processing.

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

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

Analysis of Pollutants for the Sustainable Reuse of Waste Lubricant Oils

Nowadays, attention to the environment is increasingly emphasized by the scientific community. Different measures have been adopted to ensure a lower environmental impact and increase the sustainability of industrial processes. This work fits well with these principles, as it focuses on the determination of pollutants in waste lubricating oils derived from the industrial and automotive sectors to quantify their concentration for potential recovery and subsequent reuse. Modern waste oils, especially those derived from industrial processes, contain pollutants and metals (most importantly, silicon). It is of utmost importance to determine the silicon content in the collected waste oils to verify the possibility of recycling them since high concentrations can badly affect the industrial operations in which they can be involved. One of the most applied analytic methods for controlling the content of metals is the ASTM D5185-18, Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). However, this method was certified for 50 mg/kg of maximum silicon content. To extend this range, CONOU, because of its duty to monitor waste oil quality, organized an interlaboratory comparison to verify the applicability of ASTM D5185-18 and also to samples of used oils containing higher concentrations of silicon. This work describes the details of the employed methodology and the results of the interlaboratory comparison that showed the applicability of ASTM D5185-18 also to samples containing silicon concentrations higher than 1000 ppm.

Trace elements in bean-to-bar chocolates from Brazil and Ecuador

BackgroundThe high quality and unique flavor and aroma of bean-to-bar chocolates have resulted in an increase in the consumption of these products. Nevertheless, cocoa beans may present inorganic contaminants from environmental and anthropogenic sources which can contribute to contamination of the chocolates, despite the fewer processing steps and few ingredients used in bean-to-bar manufacturing process compared to the industrial one. Therefore, this study aimed to evaluate the content of trace elements (As, Cd, Co, Cu, Hg, Pb, Se) in bean-to-bar chocolates and traceable cocoa beans from Brazil and Ecuador. MethodsBean-to-bar chocolate samples were acquired in Brazil (n=65) and Ecuador (n=10), considering the main products available: white, milk, semisweet and dark chocolate. Cocoa samples from dedicated farms (n=23) were analyzed for trace elements and inorganic contaminants regulated by Brazil and European agencies. Samples were mineralized using acid digestion (nitric acid and hydrogen peroxide) in a closed microwave-assisted system. Quantification of trace elements was performed using Inductively coupled plasma mass spectroscopy (ICP-MS) and Inductively coupled plasma optical emission spectroscopy (ICP OES) in optimized conditions. The analytical control was performed with certified reference materials (ERM BD512 - Dark Chocolate, Tort-2 and Tort-3 - Lobster Hepatopancreas and SRM 1547 - Peach leaves) and recoveries ranged between 84% and 105% for all elements. ResultsThe trace element levels in the bean-to-bar chocolates were (mg/kg): As (<0.022–0.023), Cd (<0.002–0.74), Cu (0.11–21.2), Co (<0.003–1.88), Hg (<0.010-<0.010), Pb (<0.007–0.22), and Se (<0.029–0.35). The exposure assessment from inorganic contaminants in chocolates revealed up to 93% of provisional tolerable monthly intake (PTMI) for Cd and 123% of tolerable upper intake level (UL) for Co for children. Inorganic contaminants were also analyzed in cocoa beans from dedicated farms and Cd and Pb levels were found above the thresholds established by Brazil health agency. ConclusionThe results observed for both bean-to-bar chocolates and raw materials (cocoa beans from dedicated farms) indicated a need for monitoring these trace elements.

Synthesis and Characterization of New Nanohybrids Based on Carboxymethyl Scleroglucan and Silica Nanoparticles.

In this study, two new nanohybrids (NH-A and NH-B) were synthesized through carbodiimide-assisted coupling. The reaction was performed between carboxymethyl-scleroglucans (CMS-A and CMS-B) with different degrees of substitution and commercial amino-functionalized silica nanoparticles using 4-(dimethylamino)-pyridine (DMAP) and N,N'-dicyclohexylcarbodiimide (DCC) as catalysts. The morphology and properties of the nanohybrids were investigated by using transmission (TEM) and scanning electron microscopy (SEM), electron-dispersive scanning (EDS), attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FT-IR), X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), inductively coupled plasma atomic emission spectroscopy (ICP-OES), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and dynamic light scattering (DLS). The nanohybrids exhibited differences in structure due to the incorporation of polyhedral oligomeric silsesquioxane (POSS) materials. The results reveal that hybrid nanomaterials exhibit similar thermal properties but differ in morphology, chemical structure, and crystallinity properties. Finally, a viscosity study was performed on the newly obtained nanohybrid materials; viscosities of nanohybrids increased significantly in comparison to the carboxymethyl-scleroglucans, with a viscosity difference of 7.2% for NH-A and up to 32.6% for NH-B.

Phytoremediation of pollutants in oil-contaminated soils by Alhagi camelorum: evaluation and modeling

Phytoremediation is a cost-effective and environmentally friendly method, offering a suitable alternative to chemical and physical approaches for the removal of pollutants from soil. This research explored the phytoremediation potential of Alhagi camelorum, a plant species, for total petroleum hydrocarbons (TPHs) and heavy metals (HMs), specifically lead (Pb), chromium (Cr), nickel (Ni), and cadmium (Cd), in oil-contaminated soil. A field-scale study spanning six months was conducted, involving the cultivation of A. camelorum seeds in a nursery and subsequent transplantation of seedlings onto prepared soil plots. Control plots, devoid of any plants, were also incorporated for comparison. Soil samples were analyzed throughout the study period using inductively coupled plasma-optical emission spectroscopy (ICP‒OES) for HMs and gas chromatography‒mass spectrometry (GC‒MS) for TPHs. The results showed that after six months, the average removal percentage was 53.6 ± 2.8% for TPHs and varying percentages observed for the HMs (Pb: 50 ± 2.1%, Cr: 47.6 ± 2.5%, Ni: 48.1 ± 1.6%, and Cd: 45.4 ± 3.5%). The upward trajectory in the population of heterotrophic bacteria and the level of microbial respiration, in contrast to the control plots, suggests that the presence of the plant plays a significant role in promoting soil microbial growth (P < 0.05). Moreover, kinetic rate models were examined to assess the rate of pollutant removal. The coefficient of determination consistently aligned with the first-order kinetic rate model for all the mentioned pollutants (R2 > 0.8). These results collectively suggest that phytoremediation employing A. camelorum can effectively reduce pollutants in oil-contaminated soils.

Characterization of mineral composition of leaves and flowers of wild-growing Sambucus nigra.

The objective of this study was to determine the mineral content in the leaves and flowers of wild-grown Sambucus nigra collected from eleven different locations in Kosovo. The samples were digested in a microwave system using the wet digestion method. The minerals were determined by the application of inductively coupled plasma-atomic emission spectrometry (ICP-AES) and inductively coupled plasma-mass spectrometry (ICP-MS). A total of 31 elements were determined, 15 elements by the ICP-AES method (Al, B, Ba, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, Sr, V, and Zn) and 16 elements by the ICP-MS method (Ag, As, Be, Bi, Cd, Co, Cs, Ga, Hg, In, Li, Ni, Pb, Rb, Tl, and U). The leaves of S. nigra show a higher content of minerals compared to the flowers, except for the flower of the sample SN-FL10, which is characterized by a high concentration of Fe, Al, Pb, Be, and Tl. The concentration of heavy metals and toxic elements (Pb, Cd, and Hg) was within the permissible concentrations according to Eur. Ph.

Lunar simulant behaviour in molten fluoride salt for ISRU applications

This study investigated the behaviour of a lunar mare crystalline analog dissolved in molten LiF–NaF at 800 °C for the in situ production of metals as a part of In Situ Resource Utilization (ISRU) research. Molten fluorides have the capability to dissolve metallic oxides, and the Hall-Héroult process uses this kind of media to produce Al from Al2O3.The first step was to compare the individual solubility of the main oxides composing the mare lunar soil (SiO2, Al2O3, Fe2O3, and MgO) with the solubility of the crystalline analog using Inductively Coupled Plasma – Atomic Emission Spectroscopy (ICP-AES). The species concentration added jointly are lower than the concentration of the same species added separately. Nonetheless, this study showed that LiF–NaF can be used to dissolve the analog with a maximum solubility of 3.9 wt% at 800 °C. Cyclic voltammograms were also used to verify the electroactivity of all oxide species in LiF–NaF, wherein all the main oxides are electroactive except SiO2 and TiO2. Then electrolyses on different cathodic substrates were performed at different conditions and the obtained cathodic products were analysed with a scanning electron microscope (SEM) coupled with an energy dispersive spectroscopy (EDS). Despite the non-electroactivity of SiO2 and TiO2, they were extracted in an alloyed form through Under Potential Deposition (UPD). Metallic deposition of other metals such as aluminium and titanium was achieved on carbon electrode. Finally, a synthetic mixture made of the different oxide species with the same chemical composition as the simulant, was investigated as a viable substitute for lunar mare soil. Its electrochemical behaviour was identical to the crystalline lunar simulant showing that our original process based on oxides dissolution is not influenced by the amorphous/crystalline state of the raw material.the outputs of LiF–NaF molten process are not critically influenced by the physical state of the lunar regolith.

Metal-Free Activation of Molecular Oxygen by Quaternary Ammonium-Based Ionic Liquid: A Detail Mechanistic Study.

Most oxidation processes in common organic synthesis and chemical biology require transition metal catalysts or metalloenzymes. Herein, we report a detailed mechanistic study of a metal-free oxygen (O2) activation protocol on benzylamine/alcohols using simple quaternary alkylammonium-based ionic liquids to produce products such as amide, aldehyde, imine, and in some cases, even aromatized products. NMR and various control experiments established the product formation and reaction mechanism, which involved the conversion of molecular oxygen into a hydroperoxyl radical via a proton-coupled electron transfer process. Detection of hydrogen peroxide in the reaction medium using colorimetric analysis supported the proposed mechanism of oxygen activation. Furthermore, first-principles calculations using density functional theory (DFT) revealed that reaction coordinates and transition state spin densities have a unique spin conversion of triplet oxygen leading to formation of singlet products via a minimum energy crossing point. In addition to DFT, domain-based local pair natural orbital coupled cluster, (DLPNO-CCSD(T)), and complete active space self-consistent field, CASSCF(20,14) methods complemented the above findings. Partial density of states analysis showed stabilization of π* orbital of oxygen in the presence of ionic liquid, making it susceptible to hydrogen abstraction in a mild, metal-free condition. Inductively coupled plasma atomic emission spectroscopic (ICP-AES) analysis of reactant and ionic liquids clearly showed the absence of any significant transition metal contamination. The current results described the origin of O2 activation within the context of molecular orbital (MO) theory and opened up a new avenue for the use of ionic liquids as inexpensive, multifunctional and high-performance alternative to metal-based catalysts for O2 activation.