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The thermally stable zirconium-based MOF, UiO-66, was employed for the preparation of bonded porous-layer open-tubular (PLOT) GC columns. The synthesis included the in situ growth of the UiO-66 film on the inner wall of the capillary through a one-step solvothermal procedure. SEM-EDX analysis revealed the formation of a thin, continuous, uniform, and compact layer of UiO-66 polycrystals on the functionalized inner wall of the column. The average polarity (ΔIav = 700) and the McReynolds constants reflected the polar nature of the UiO-66 stationary phase. Several mixtures of small organic compounds and real samples were used to evaluate the separation performance of the fabricated columns. Linear alkanes from n-pentane to n-decane were baseline separated within 1.35 min. Also, a series of six n-alkylbenzenes (C3-C8) were separated within 3 min with a minimum resolution of 3.09, whereas monohalobenzene mixtures were separated at 220 °C within 14s. UiO-66 PLOT columns are ideally suited for the isothermal separation of chlorobenzene structural isomers at 210 °C within 45 s with Rs ≥ 1.37. The prepared column featured outstanding thermal stability (up to 450 °C) without any observed bleeding or significant impact on its performance. This feature enabled the analysis of various petroleum-based samples.
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Recycling waste from the production and consumption of heat-resistant alloys to return them to production is an urgent task due to the high cost of the components contained in these alloys. The kinetics and conditions of the acid leaching process of the grinding waste of a heat-resistant nickel alloy are studied depending on the composition of the acid solution (H2SO4, HCl, HNO3, and their mixtures) at room temperature to boiling point temperature and various acid concentrations (1.5 to 3.0 mol/L), ratios of waste to solution (1:10 to 3:10), fraction sizes (0.04-1 mm), and contact duration (1 to 120 h). The linearization of experimental data by the Gray-Weddington, Gistling-Brownstein, and Kazeev-Erofeev equations showed that the rate of the leaching process was influenced by both the chemical reactions between sulfuric acid and metals included in the grinding waste and the diffusion of reagents through the film of reaction products and undissolved impurities. Optimal conditions for acid dissolution of the grinding waste have been established to obtain the maximum degree of extraction of the main component of the alloy, nickel. The processing of powder particles with a size of less than 0.1 mm should be carried out in a solution of sulfuric acid with a concentration of 3.0 mol/L at a temperature of 100 °C for 6 h with a ratio of solid to liquid phases of 1:10. The reported results are very important for industry personnel to recover metals and for environmentalists to treat the alloy waste.
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Municipal wastewater contains emergent chemical and biological pollutants that are resistant to conventional wastewater treatments. Therefore, the focus of the current study was to address the challenge of removing emergent chemical and biological pollutants present in municipal wastewater. To achieve this, a photo electro-catalytic (PEC) treatment approach was employed, focusing on the removal of both micro and biological pollutants that are of emergent concern, as well as the reduction of Chemical Oxidation Demand (COD) and Total Organic Carbon (TOC). The treatment involved the use of a modified multi-layer catalytic anode photo-electroactive anode as an effective anode for PEC treatment of municipal wastewater. In the continuous mode of operation, %COD removal was optimized for the treatment of municipal wastewater under Ultra-Violet C (UVc), 280 nm, and Visible (Vis) radiation, 400 nm. Therefore, a comparative study was performed to investigate the effect of Vis radiation on %COD removal, micropollutants removal, and disinfection of municipal wastewater. Micropollutants present in municipal wastewater were effectively oxidized/degraded with the highest reduction rate between 100% and 80% under the influence of UVc and Vis radiation respectively by the PEC treatment process. Disinfection of various microorganisms present in the wastewater with the effect of UVc and Vis assisted PEC treatment was also monitored. Overall, 75-80% of the disinfection of municipal wastewater was contributed by the modified multi-layer catalytic anode. The UVc in the PEC system, contributes approximately 20-25% to the overall disinfection of municipal wastewater.
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Contaminantes Ambientales , Contaminantes Químicos del Agua , Aguas Residuales , Contaminantes Químicos del Agua/química , Oxidación-Reducción , ElectrodosRESUMEN
Contemporary food marketing is ruined by flavor enhancers rather than emphasizing the nutritional value of food. Vanillin is an overexploited flavor enhancer added to food items, thereby necessitating its detection. In this study, an electrochemical sensor was designed using a modified electrode made up of La2NiO4 functionalized carbon nanofiber (f-CNF) to effectively detect vanillin in food samples. To confirm the successful formation of La2NiO4/f-CNF, structural and morphological studies were performed using X-ray diffraction, Raman spectroscopy, scanning electron microscopy, and X-ray photoelectron spectroscopy. Further electrochemical analysis was performed using cyclic voltammetry and differential pulse voltammetry techniques, which resulted in high sensitivity (0.2899 µA·µM-1·cm-2) and low limit of detection (LOD) (6 nM). This modified electrode material was tested in food samples, which showed an excellent response with recovery percentage and is a promising electrocatalyst for vanillin detection.
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Carbono , Nanofibras , Carbono/química , Lantano , Aditivos Alimentarios , Nanofibras/química , Técnicas Electroquímicas/métodos , ElectrodosRESUMEN
Phthalates are synthetic chemicals widely used, mainly as plasticizers, which are ubiquitous and recognized as endocrine-disrupting chemicals. For investigation of phthalate residues leached from PET bottles into drinking water, a simple and sensitive method was developed, validated and applied to a series of real samples. Solid-phase microextraction (SPME) was used in direct immersion mode for concentration of phthalate traces from 10 mL of each water sample. Four commercially available SPME fibers were tested and compared, while six dialkyl phthalates were investigated: dimethyl phthalate (DMP), diethyl phthalate (DEP), diisopropyl phthalate (DiPP), diisobutyl phthalate (DiBP), di-n-butyl phthalate (DnBP) and di-ethylhexyl phthalate (DEHP). The extracted phthalic acid esters were separated and quantified by gas chromatography hyphenated with tandem mass spectrometry (GC-MS/MS) and a detection method based on multiple reaction monitoring (MRM) mode was fully developed, optimized and validated. The fiber which showed the highest ability for extraction of phthalates was DVB/CAR/PDMS which combines a liquid polymeric coating (polydimethyl siloxane and divinylbenzene) with a carboxen porous sorbent layer. The obtained limit of detection was in the range between 0.3 and 2.6 ng mL-1. Thus, this fiber was used for extraction of phthalates from twelve commercial PET bottled water samples. All investigated water brands showed the presence of two to six phthalates at concentrations between 6.3 and 112.2 ng mL-1. The highest level was observed for DnBP, followed by DEHP, DiBP, DMP, DEP and DiPP.
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Dietilhexil Ftalato , Agua Potable , Ácidos Ftálicos , Dietilhexil Ftalato/análisis , Agua Potable/química , Cromatografía de Gases y Espectrometría de Masas/métodos , Ácidos Ftálicos/análisis , Microextracción en Fase Sólida , Espectrometría de Masas en TándemRESUMEN
In this work, we developed a simple spectrophotometric strategy for BrO3- ions determination as a major water disinfection constituents in the mice's liver tissues by using pararosaniline (PRA). Mice were divided into seven main groups (6 doses): lowest dose KBrO3 (G1 0.01 mg L-1, G2 0.025 mg L-1 and G3 0.1 mg L-1), highest dose KBrO3 (G4 1 mg L-1, G5 10 mg·L-1 and G6 30 mg L-1) and control. All these groups maintained a dose-specific feeding for one month, just before the bromate assessment in mice's liver samples. The results revealed that groups of exposure to lower doses of drinking water did not detect the presence of BrO3- accumulated in the liver tissue during the study period (1-2 months). While, the BrO3- was detected in higher dosages for samples analyzed in first, second, third, fourth and fifth weeks (W1, W2, W3, W4, and W5). These results confirmed that the higher BrO3- dosages (1, 10, and 30 mg L-1) were fatal if introduced in drinking water and could accumulate in the liver tissues both for mice and for human. Detection the accuracy of the method for recovery of bromate ions in liver samples (N = 5) was found to be more than 95%. Relative standard deviations (RSDs) were found to be less than 2.0% confirming the reproducibility of the assay technique.
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Bromatos , Hígado , Administración Oral , Animales , Bromatos/toxicidad , Masculino , Ratones , Reproducibilidad de los ResultadosRESUMEN
An ultra high performance liquid chromatography-tandem mass spectrometric method has been developed for the highly sensitive and selective determination of regulated aflatoxins. The extraction of aflatoxins from baby food matrices were performed using liquid-liquid extraction procedure followed by immunoaffinity column cleanup. The higher sensitivity for the determination of target aflatoxins was fulfilled by applying a preconcentration step with immunoaffinity columns after acetonitrile-water extraction. The enhanced selectivity was attained with the triple quadrupole mass analyzer operated in electrospray positive ionization mode. Method validation was tested in five different baby food matrices by recovery experiments. Satisfactory recoveries, between 92 and 103%, with relative standard deviations lower than 8% were achieved in all the tested matrices. The proposed method was found to be specific as no interference peaks were observed for blank samples. The limit of detection of the method was found to be in the range of 0.003-0.008 ng/mL. The validated method was fruitfully applied to the screening of aflatoxins in baby foods and feeds sample retailed in local markets of Riyadh, Saudi Arabia. The obtained levels of all analyzed aflatoxins were below the regulation limits set by European Agency.
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Aflatoxinas/análisis , Contaminación de Alimentos/análisis , Alimentos Infantiles/análisis , Cromatografía de Afinidad , Cromatografía Líquida de Alta Presión , Humanos , Lactante , Estructura Molecular , Espectrometría de Masas en TándemRESUMEN
Efforts to improve water quality have led to the development of green and sustainable water treatment approaches. Herein, nitrogen-doped magnetized hydrochar (mSBHC-N) was synthesized, characterized, and used for the removal of post-transition and transition heavy metals, viz. Pb2+ and Cd2+ from aqueous environment. mSBHC-N was found to be mesoporous (BET surface area - 62.5â¯m2/g) and paramagnetic (saturation magnetization - 44 emu/g). Both, FT-IR (with peaks at 577, 1065, 1609 and 3440â¯cm-1 corresponding to Fe - O stretching vibrations, C - N stretching, N - H in-plane deformation and stretching) and XPS analyses (with peaks at 284.4, 400, 530, 710â¯eV due to C 1s, N 1s, O 1s, and Fe 2p) confirmed the presence of oxygen and nitrogen containing functional groups on mSBHC-N. The adsorption of Pb2+ and Cd2+ was governed by oxygen and nitrogen functionalities through electrostatic and co-ordination forces. 75-80% of Pb2+ and Cd2+ adsorption at Co: 25â¯mg/L, either from deionized water or humic acid solution was accomplished within 15â¯min. The data was fitted to pseudo-second-order kinetic and Langmuir isotherm models, with maximum monolayer adsorption capacities being 323 and 357â¯mg/g for Cd2+and Pb2+ at 318â¯K, respectively. Maximum Cd2+ (82.6%) and Pb2+ (78.7%) were eluted with 0.01â¯M HCl, simultaneously allowing minimum iron leaching (2.73%) from mSBHC-N. In conclusion, the study may provide a novel, economical, and clean route to utilize agro-waste, such as sugarcane bagasse (SB), for aquatic environment remediation.
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Magnetismo/métodos , Metales Pesados/química , Contaminantes Químicos del Agua/química , Purificación del Agua/métodos , Agua/química , Adsorción , Contaminantes Químicos del Agua/análisisRESUMEN
Modern-day practices are the major contributors in water quality deterioration, consequently results in clean water scarcity. Herein, co-precipitation procedure was adopted to develop a nanomagnetic copper ferrite/drumstick pod biomass (CuFe2O4/DC) composite, which was characterized, and optimized to sequester malachite green (MG) and lead (Pb(II)) in unary and binary systems from aqueous environment. Mesoporous CuFe2O4/DC surface with 16.96 m2/g BET surface area and acid functionalities predominance was observed. Under the studied experimental conditions, MG adsorption on CuFe2O4/DC in unary system was comparatively higher than that of Pb(II). MG and Pb(II) equilibrium results were fitted to Langmuir isotherm model, their respective maximum monolayer adsorption capacities at 328 K being 952.4 and 921.1 mg/g. On the other hand, binary system (in presence of MG) fastened Pb(II) adsorption kinetics and increased its uptake capacity. Additionally, humic acid (HA) matrix enhanced Pb(II) adsorption kinetics. Recovery studies showed maximal MG and Pb(II) elution with C2H5OH and 0.1 mol/L HCl, respectively. An 82.7% drop in Pb(II) adsorption was found after the first regeneration cycle, while only 17.6% fall in MG adsorption was witnessed after five consecutive regeneration cycles. Hence, it could be concluded that CuFe2O4/DC is a cost-effective and promising adsorbent for an efficient and rapid removal of Pb(II) and MG from both unary and binary systems.
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Biomasa , Cobre/química , Compuestos Férricos/química , Plomo/química , Nanotecnología , Colorantes de Rosanilina/química , AdsorciónRESUMEN
The present study reports the outcomes of assessment on acrylamide levels in selected heat-treated foods of diverse brands and origins from Saudi Arabia. In chips, acrylamide level was detected from 28 to 954 µg/kg, sample 7 (salted) contained higher amount (954 µg/kg) whereas, sample 8 (labneh and mint) comparatively produced lower amount (28 µg/kg). Nuts and dried fruits have generated acrylamide from 2 to 93 µg/kg, salted peanut of Indian origin produced higher amount (93 µg/kg) while apricot (plain) relatively generated lower amount (2 µg/kg). The levels of acrylamide in biscuits, pastry, cacao, chocolate, olive, cheese, corn, oat and wheat flakes, and bread were found from 26 to 234 µg/kg. Biscuits generated high concentration (234 µg/kg) while corn flakes fairly generated lower amount (26 µg/kg). The obtained results have shown a great variation of acrylamide content and reason might be due to foods type, cooking ingredients and, cooking methods, time and temperature.
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The combination of magnetic nanoparticles and metal-organic frameworks (MOFs) has demonstrated their prospective for pollutant sequestration. In this work, a magnetic metal-organic framework nanocomposite (Fe3O4@AMCA-MIL53(Al) was prepared and used for the removal of U(VI) and Th(IV) metal ions from aqueous environment. Fe3O4@AMCA-MIL53(Al) nanocomposite was characterized by TGA, FTIR, SEM-EDX, XRD, HRTEM, BET, VSM (vibrating sample magnetometry), and XPS analyses. A batch technique was applied for the removal of the aforesaid metal ions using Fe3O4@AMCA-MIL53(Al) at different operating parameters. The isotherm and kinetic data were accurately described by the Langmuir and pseudo-second-order models. The adsorption capacity was calculated to be 227.3 and 285.7 mg/g for U(VI) and Th(IV), respectively, by fitting the equilibrium data to the Langmuir model. The kinetic studies demonstrated that the equilibrium time was 90 min for each metal ion. Various thermodynamic parameters were evaluated which indicated the endothermic and spontaneous nature of adsorption. The collected outcomes showed that Fe3O4@AMCA-MIL53(Al) was a good material for the exclusion of these metal ions from aqueous medium. The adsorbed metals were easily recovered by desorption in 0.01 M HCl. The excellent adsorption capacity and the response to the magnetic field made this novel material an auspicious candidate for environmental remediation technologies.
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A substantive approach converting waste date pits to mercerized mesoporous date pit activated carbon (DPAC) and utilizing it in the removal of Cd(II), Cu(II), Pb(II), and Zn(II) was reported. In general, rapid heavy metals adsorption kinetics for Co range: 25-100 mg/L was observed, accomplishing 77-97% adsorption within 15 min, finally, attaining equilibrium in 360 min. Linear and non-linear isotherm studies revealed Langmuir model applicability for Cd(II) and Pb(II) adsorption, while Freundlich model was fitted to Zn(II) and Cu(II) adsorption. Maximum monolayer adsorption capacities (qm) for Cd(II), Pb(II), Cu(II), and Zn(II) obtained by non-linear isotherm model at 298 K were 212.1, 133.5, 194.4, and 111 mg/g, respectively. Kinetics modeling parameters showed the applicability of pseudo-second-order model. The activation energy (Ea) magnitude revealed physical nature of adsorption. Maximum elution of Cu(II) (81.6%), Zn(II) (70.1%), Pb(II) (96%), and Cd(II) (78.2%) were observed with 0.1 M HCl. Thermogravimetric analysis of DPAC showed a total weight loss (in two-stages) of 28.3%. Infra-red spectral analysis showed the presence of carboxyl and hydroxyl groups over DPAC surface. The peaks at 820, 825, 845 and 885 cm-1 attributed to Zn-O, Pb-O, Cd-O, and Cu-O appeared on heavy metals saturated DPAC, confirmed their binding on DPAC during the adsorption.
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Metales Pesados/aislamiento & purificación , Phoeniceae , Contaminantes Químicos del Agua/aislamiento & purificación , Purificación del Agua/instrumentación , Adsorción , Cadmio/aislamiento & purificación , Carbono/química , Cobre/aislamiento & purificación , Concentración de Iones de Hidrógeno , Cinética , Plomo/aislamiento & purificación , Termogravimetría , Zinc/aislamiento & purificaciónRESUMEN
In this study, the determination of noxious heavy metals, cadmium (Cd), bismuth (Bi), mercury (Hg), titanium (Ti), lead (Pb) and metalloid arsenic (As) in skin-whitening cosmetics were examined using microwave digestion and inductively coupled plasma atomic emission spectrometry method. A complete digestion of cosmetics samples was achieved using a mixture of hydrofluoric acid/hydrogen peroxide/nitric acid. The quantification of the target compounds was done by standard addition method. The excellent quality parameters for instance, detection limits, As (4.6â ppb), Bi (7.9â ppb), Cd (0.45â ppb), Hg (3.3â ppb), Pb (3.8â ppb), Ti (4.3â ppb), linearity (r2 > 0.999) and run-to-run and day-to-day precisions with relative standard deviations <3% were obtained. The recovery rates for standard reference materials were found between 90 and 105%. The average concentration of heavy metals in cosmetics samples were in the range of 1.0-12.3 (µgâ g-1, As), 33-7097 (µgâ g-1, Bi), 0.20-0.6 (µgâ g-1, Cd), 0.70-2700 (µgâ g-1, Hg), 1.20-143 (µgâ g-1, Pb) and 2.0-1650 (µgâ g-1, Ti).
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Cosméticos/química , Metales Pesados/análisis , Preparaciones para Aclaramiento de la Piel/química , Análisis Espectral/métodos , Humanos , Límite de Detección , Microondas , Estándares de ReferenciaRESUMEN
With the aim of preparing high performance oxide-dispersion-strengthened tungsten based alloys by powder metallurgy, the W-Y2O3 composite nanopowder precursor was fabricated by an improved wet chemical method with anion surfactant sodium dodecyl sulfate (SDS) addition. It is found that the employment of SDS can dramatically decrease W grain size (about 40 nm) and improve the size uniformity. What's more, SDS addition can also remarkably improve the uniform dispersion of Y2O3 particles during the synthesis process. For the alloy whose powder precursor was fabricated by traditional wet chemical method without SDS addition, only a few Y2O3 dispersoids with size of approximate 10-50 nm distribute unevenly within tungsten grains. Nevertheless, for the sintered alloy whose powder precursor was produced by improved wet chemical method, the Y2O3 dispersoids (about 2-10 nm in size) with near spherical shape are dispersed well within tungsten grains. Additionally, compared with the former, the alloy possesses smaller grain size (approximate 700 nm) and higher relative density (99.00%). And a Vickers microhardness value up to 600 Hv was also obtained for this alloy. Based on these results, the employment of SDS in traditional wet chemical method is a feasible way to fabricate high performance yttria-dispersion-strengthened tungsten based alloys.
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A series of porous carbon spheres with precisely adjustable mesopores (4-16 nm), high specific surface area (SSA, â¼2000 m2 g-1), and submicrometer particle size (â¼300 nm) was synthesized through a facile coassembly of diblock polymer micelles with a nontoxic dopamine source and a common postactivation process. The mesopore size can be controlled by the diblock polymer, polystyrene-block-poly(ethylene oxide) (PS-b-PEO) templates, and has an almost linear dependence on the square root of the degree of polymerization of the PS blocks. These advantageous structural properties make the product a promising electrode material for electrochemical capacitors. The electrochemical capacitive performance was studied carefully by using symmetrical cells in a typical organic electrolyte of 1 M tetraethylammonium tetrafluoroborate/acetonitrile (TEA BF4/AN) or in an ionic liquid electrolyte of 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIMBF4), displaying a high specific capacitance of 111 and 170 F g-1 at 1 A g-1, respectively. The impacts of pore size distribution on the capacitance performance were thoroughly investigated. It was revealed that large mesopores and a relatively low ratio of micropores are ideal for realizing high SSA-normalized capacitance. These results provide us with a simple and reliable way to screen future porous carbon materials for electrochemical capacitors and encourage researchers to design porous carbon with high specific surface area, large mesopores, and a moderate proportion of micropores.
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Highly ordered mesostructured vanadium phosphonates (VP) have been synthesized in the presence of cetyltrimethylammonium bromide (CTAB) as a structure-directing agent. Nitrilotris(methylene)triphosphonic acid (NMPA) and (ammonium/sodium) metavanadate (NH4 VO3 /NaVO3 ) have been used for the construction of pore walls. The CTAB templates are removed from the materials by an extraction process without destroying the parent mesostructure. The formation mechanism for the ordered mesoporous structure and its impact on electrochemical application in lithium ion batteries (LIBs) are explained by considering the structural and electrochemical stability of the framework. The results demonstrate that the counter cations (NH4+ /Na+ ) of the metavanadate precursors have a crucial role in stabilizing the mesoporous structure of the mesoporous VP materials. Mesoporous VP materials with highly ordered structure have great applicability as high-performance electrode materials in LIBs due to the advantages of their large contact area with electrolyte and short transport paths for lithium ions. Mesoporous VP electrodes exhibit high reversible specific capacity with superb cycling stability (100â cycles) and excellent retention of capacity (92 %).
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The present work describes the outcomes of the assessment on acrylamide contents in a number of thermally treated foods (Arabic coffee Qahwa, coffee and tea) obtained from the Saudi Arabian markets. A total of 56 food samples of different brands and origin were studied, the amounts of acrylamide in Arabic coffee Qahwa, coffee and tea were obtained in the range of 10 to 682 µg kg-1. In comparison to coffee (152-682 µg kg-1), the Arabic coffee Qahwa (73-108 µg kg-1) and tea (10-97 µg kg-1) contain lower amounts of acrylamide. Among the analyzed samples, the green tea contained low amounts of acrylamide ranged from 10 to 18 µg kg-1, and thus the green tea could be considered as a healthier hot drink. A great variation of acrylamide formation has been observed in these food products. This divergence may be due to the initial concentration of amino acids especially asparagines and reducing sugars in food products, in addition to roasting temperature and time, pH and water activity. The obtained data can also be used in epidemiological investigation to estimate the acrylamide exposure from nutritional survey.
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Acrilamida/análisis , Carcinógenos/análisis , Café/química , Contaminación de Alimentos , Té/química , Café/normas , Arabia Saudita , Té/normasRESUMEN
To develop low-cost and efficient oxygen reduction reaction (ORR) catalysts, a novel hybrid comprising cobalt-embedded nitrogen-doped carbon nanotubes and nitrogen-doped reduced graphene oxide (Co-NCNT/NrGO-800) was simply prepared by pyrolysis. The combination of nanotubes and graphene, and the efficient doping with cobalt and nitrogen, greatly contribute to the excellent ORR performance. This optimized Co-NCNT/NrGO catalyst exhibits a positive onset potential of 0.91â V and a half-wave potential of 0.82â V, combined with a relatively low peroxide yield, better durability, and better methanol tolerance than commercially available Pt/C, which makes it a promising candidate as a low-cost and effective non-precious-metal ORR catalyst.
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A simple, fast, highly efficient and direct method using ultra-performance liquid chromatography coupled to mass spectrometry has been established for the simultaneous separation, identification and quantitation of a few saturated and unsaturated fatty acids in olive oils from various countries. No sample pretreatment techniques were employed such as extraction or derivatization for the analysis of target acids from oil samples, as the oil samples were just diluted, filtered and then directly injected to the instrument. The chromatographic separations of all target fatty acids were achieved on a Hypersil Gold C18 column of particle size 1.9µm, 50×2.1mm I.D, while the gradient elution using a binary mobile phase mixture of acetonitrile and water at a flow rate of 1.5ml/min was adopted for achieving optimum separations. The identification and quantitation of target compounds was accomplished using selected ion reaction monitoring mode. The recoveries of the fatty acids were obtained higher than 89% with good validation parameters; linearity (r(2)>0.992), detection limit between 0.09 and 0.24µg/ml, run to run and day to day precisions with percent relative standard deviation lower than 2.4% at both low (1µg/ml) and medium (10µg/ml) concentration levels. The total content of fatty acids in each individual oils was found in the range of 472.63-7751.20µg/ml of olive oil, while oleic acid was found to be the major fatty acid among all analyzed oils with the amount 3785.94µg/ml (maximum) in Syrian olive oil. The obtained validation parameters confirm that the proposed analytical method is rapid, sensitive, reproducible and simple and it could be applied for the successful evaluation of fatty acids in various oils and other matrices. All the fatty acids were efficiently eluted in a time of less than 8min with well resolved peaks by employing the proposed method.
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Cromatografía Líquida de Alta Presión/métodos , Ácidos Grasos no Esterificados/análisis , Espectrometría de Masas/métodos , Aceite de Oliva/química , Calibración , Reproducibilidad de los ResultadosRESUMEN
Engineering the size, composition, and morphology of platinum-based nanomaterials can provide a great opportunity to improve the utilization efficiency of electrocatalysts and reinforce their electrochemical performances. Herein, three-dimensional platinum-palladium hollow nanospheres with a dendritic shell (PtPd-HNSs) are successfully fabricated through a facile and economic route, during which SiO2 microspheres act as the hard template for the globular cavity, whereas the triblock copolymer F127 contributes to the formation of the dendritic shell. In contrast with platinum hollow nanospheres (Pt-HNSs) and commercial platinum on carbon (Pt/C) catalyst, the novel architecture shows a remarkable activity and durability toward the methanol oxidation reaction (MOR) owing to the coupled merits of bimetallic nanodendrites and a hollow interior. As a proof of concept, this strategy is also extended to trimetallic gold-palladium-platinum hollow nanospheres (AuPdPt-HNSs), which paves the way towards the controlled synthesis of other bi- or multimetallic platinum-based hollow electrocatalysts.