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The deposition of TiN on stainless steel substrates may improve the stability and compatibility of this material with bone, which may be advantageously exploited for the elaboration of advanced pros- thetic devices. In this work, TiN-coated 316LSS (by way of DC magnetron sputtering) was used as a starting material for investigating the electrochemical post-deposition of hydroxyapatite (HAp) which has a composition close to that of bone. Electrodeposition was carried out starting from an aqueous medium containing solubilized Ca(NO3)2 and NH4H2PO4 in the presence of H2O2. We report the influence of experimental conditions on the morphology of the obtained HAp coating on TiN/316LSS. The effect of applied potential, temperature, H2O2 concentration, pH and duration of reaction were thoroughly discussed on the basis of X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and Energy Dispersive X-ray Spectroscopy (EDX) results. This method appears advantageous for producing HAp-coated implant materials.
Assuntos
Materiais Biocompatíveis/química , Durapatita/química , Titânio/química , Galvanoplastia , Peróxido de Hidrogênio , Microscopia Eletrônica de Varredura , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios XRESUMO
In this study, CoCr layered double hydroxide material (CoCr-LDH) was prepared and used as an effective catalyst for peroxymonosulfate (PMS) activation to degrade organics in water. The prepared CoCr-LDH material had a crystalline structure and relatively porous structure, as determined by various surface analyses. In Rhodamine B (RhB) removal, the most outstanding PMS activation ability belongs to the material with a Co:Cr molar ratio of 2:1. The removal of RhB follows pseudo-first-order kinetics (R2 > 0.99) with an activation energy of 38.23 kJ/mol and efficiency of 98% after 7 min of treatment, and the total organic carbon of the solution reduced 47.2% after 10 min. The activation and oxidation mechanisms were proposed and the RhB degradation pathways were suggested with the key contribution of O2â¢- and 1O2. Notably, CoCr-LDH can activate PMS over a wide pH range of 4 - 9, and apply to a wide range of organic pollutants and aqueous environments. The material has high stability and good recovery, which can be reused for 5 cycles with a stable efficiency of above 88%, suggesting a high potential for practical recalcitrant water treatment via PMS activation by heterogeneous catalysts.
Assuntos
Peróxidos , Poluentes Químicos da Água , Purificação da Água , Poluentes Químicos da Água/química , Peróxidos/química , Purificação da Água/métodos , Rodaminas/química , Cinética , Oxirredução , CatáliseRESUMO
Photocatalysts based on titanium dioxide (TiO2) were widely applied to solve environmental problems such as water and air pollution treatment. Currently, the application of these compounds for food packaging is increasing. This study prepared silver (Ag) doped TiO2 photocatalyst (Ag/TiO2) for the decomposition of gas ethylene (Eth), which is the main factor that causes fruits to over-ripen and damage or decay. It found that the doping of Ag could improve the optical property and light adsorption ability of Ag/TiO2 photocatalyst, which directly enhanced the photocatalytic decomposition of Eth performance. Under visible light, Ag/TiO2 could depredate 91.2% of Eth, while the removal performance by using the original TiO2 was 43.9%. The increased initial concentration of Eth from 5 to 30 ppm could inhibit the photocatalytic efficiency of Ag/TiO2 from 98.6 to 69.2%. Besides, the relative humidity and gas flow rate are roles in the Eth decomposition process. The recycling experiment confirmed that Ag/TiO2 had good reusability with a slight loss in photocatalytic performance (18.6%) after ten cycles tested. The future protective application of Ag/TiO2 for food protection during storage and transportation is discussed. This work provides a potential method to remove gas ethylene, reduce the ripening process and extend the shelf life of fruits.
Assuntos
Luz , Titânio , Titânio/farmacologia , Prata/farmacologia , Etilenos , CatáliseRESUMO
A heavy-atom-free photosensitizer (CI) based on an imidazole-carbazole conjugate exhibited strong fluorescence emission and ROS generation via both type I and II mechanisms. In particular, CI showed efficient photodynamic therapy and fluorescence bioimaging under two-photon (TP) excitation (740 nm) toward HeLa cells with negligible dark toxicity.
Assuntos
Fotoquimioterapia , Humanos , Fluorescência , Células HeLa , Fotoquimioterapia/métodos , Carbazóis , ImidazóisRESUMO
In the present study, the biosynthesis of stable silver nanoparticles (BioAgNPs) was accomplished successfully for the first time by using an aqueous extract derived from the buds of Syzygium nervosum (SN) as both a reducing and a stabilizing agent. Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HR-TEM) investigations revealed that the biosynthesized BioAgNPs were predominantly spherical with an average size of 10-30 nm. It was found that the outstanding stability of the BioAgNPs colloidal solution was assigned to the additive effect of the surrounding protective organic layer and the highly negatively charged surface of the nanoparticles. Consequently, good antibacterial activity was demonstrated by the colloidal BioAgNPs solution against four distinct bacterial strains, including Gram-positive S. aureus and B. subtilis as well as Gram-negative E. coli and S. typhi. Interestingly, the biosynthesized BioAgNPs displayed greater antibacterial activity even when tested at low doses against Gram-negative S. typhi. In addition, the biogenic AgNPs demonstrated a significant level of catalytic activity in the process of converting 2-NP, 3-NP, and 4-NP into aminophenols within 15 min, with reaction rate constants of 9.0 × 10-4, 10 × 10-4, and 9.0 × 10-4 s-1, respectively. BioAgNPs formulations were assessed against anthracnose disease in tea plants and were found to be as effective as the positive control at a dose of 20-fold dilution, but less effective at a dose of 30-fold dilution. Both doses of BioAgNPs formulations significantly suppressed Colletotrichum camelliae (anthracnose disease) without affecting the growth of the tea plants.
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In this study, we fabricated a composite of NiO-ZnO/PANI-CNTs on a fluorine tin oxide (FTO) electrode and examined the electrochemical sensing behavior of the modified electrode to detect methanol in aqueous solution. The structural, morphological, and electrochemical properties of the composite were characterized using various methods such as X-ray diffraction (XRD), EDS, FTIR, X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and electrochemical techniques such as cyclic voltammetry (CV) and chronoamperometry (CA). The composite-based electrode showed excellent electrocatalytic activity and selectivity for methanol oxidation. The calibration equation obtained was ΔI = 0.0003 × CMeOH + 0.02811, with a high correlation coefficient of 0.9993, over a wide detection range of 0 to 500 mM. The material exhibits great potential for the fabrication of sensors to detect methanol in commercial products. Real gasoline samples have been selected to evaluate the practical performance and feasibility of this as-prepared sensor. The experimental data indicated that the recovery of gasoline samples is about 98%, indicating this to be an appropriate detection procedure for effective electrochemical determination of MeOH in real gasoline samples.
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This study delves into the advanced integration of a ternary heterogeneous Z-scheme photocatalyst, TiO2/CuInS2/OCN (OCN: O-g-C3N4), with carbon quantum dot (CQD) to improve the degradation efficiency of reactive yellow 145 (RY145) dye in water. Through a systematic examination, we elucidated the photocatalytic mechanisms and the role of radicals, electrons, and holes in the treatment process. Our findings revealed that this novel catalyst integration significantly boosted RY145 degradation efficiency, achieving 98.2%, which is markedly higher than the efficiencies which could be achieved using TiO2/CuInS2/OCN alone. Moreover, the TiO2/CuInS2/OCN/CQD photocatalyst demonstrated superior rate performance over its components. Comprehensive evaluations, including photoelectrochemical and radical tests, further confirmed the efficiency of the integrated system, adhering to Z-scheme principles. The catalyst showcased remarkable stability, with over 94% reusability after five reaction cycles. These findings pave the way for the potential use of the TiO2/CuInS2/OCN/CQD photocatalyst as an innovative solution for water pollutant treatment via photocatalytic technology.
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Condensation of quinaldine with 4,6-di (tert-butyl)-3-nitro-1,2-benzoquinone results in the formation of 5,7-di (tert-butyl)-2-(quinoline-2-yl)-1,3-tropolone, 5,7-di (tert-butyl)-4-nitro-2-(quinoline-2-yl)-1,3-tropolone, 3,3-dimethyl-2-(5-hydroxy-4-nitro-3-tert-butyl-6-quinoline-2-yl-pyridine-2-yl)butanoic acid, 6-(2,2-dimethylprop-3-yl)-5-tert-butyl-4-nitro-2-(quinoline-2-yl)-pyridine-3-ol, 1,7-di (tert-butyl)-3-(quinoline-2-yl)-2-azabicyclo-[3.3.0]octa-2,7-diene-4,6-dione-N-oxide. The formation of 1,3-tropolone and pyridine-2-yl butanoic acid derivatives proceeds through a ring expansion and 2-azabicyclo [3.3.0]octa-2,7-diene-4,6-dione-N-oxide via the contraction of the o-quinone ring. The structure of the heterocyclic compounds obtained was justified by X-ray diffraction analysis, NMR spectroscopy, IR- and HRMS-spectrometry, and the proposed mechanisms of their formation include the participation of an intermediate product of the expansion reaction of the o-quinone cycle - 5,7-di (tert-butyl)-4-nitro-2-(quinoline-2-yl)-cyclohepta-1,3,5-triene-1,3-diol, which was first isolated preparatively. The DFT/B3LYP/6-311++G** methods were used to determine the thermodynamic stability of tautomeric forms of intermediate products, as well as the relative stability of NH and OH tautomers of 5,7-di (tert-butyl)-2-(quinolin-2-yl)-1,3-tropolone and 5,7-di (tert-butyl)-4-nitro-2-(quinolin-2-yl)-1,3-tropolone.
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In this study, vinyltrimethoxysilane-treated hydroxyapatite (vHAP) and PMMA-grafted HAP (gHAP) were successfully prepared from original HAP (oHAP). Three kinds of HAP (oHAP, vHAP and g HAP) were used as additives for the preparation of three groups of HAP-modified PMMA bone cements (oHAP-BC, vHAP-BC and gHAP-BC). The setting, bending and compression properties of the bone cements were conducted according to ISO 5833:2002. The obtained results showed that the maximum temperature while curing the HAP-modified bone cements (HAP-BCs) decreased from 64.9 to 60.8 °C and the setting time increased from 8.1 to 14.0 min, respectively, with increasing HAP loading from 0 to 15 wt.%. The vHAP-BC and gHAP-BC groups exhibited higher mechanical properties than the required values in ISO 5833. Electron microscopy images showed that the vHAP and gHAP nanoparticles were dispersed better in the polymerized PMMA matrix than the oHAP nanoparticles. FTIR analysis indicated the polar interaction between the PO4 groups of the HAP nanoparticles and the ester groups of the polymerized PMMA matrix. Thermal gravimetric analysis indicated that mixtures of ZrO2/HAPs were not able to significantly improve the thermal stability of the HAP-BCs. DSC diagrams showed that the incorporation of gHAP to PMMA bone cement with loadings lower than 10 wt.% can increase Tg by about 2.4 °C.
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Tropolones are promising organic compounds that can have important biologic effects. We developed a series of new 2-quinolyl-1,3-tropolones derivatives that were prepared by the acid-catalyzed reaction of 4,7-dichloro-2-methylquinolines with 1,2-benzoquinones. 2-Quinolyl-1,3-tropolones have been synthesized and tested for their anti-proliferative activity against several human cancer cell lines. Two compounds (3d and mixture B of 3i-k) showed excellent activity against six cancer cell lines of different tissue of origin. The promising compounds 3d and mixture B of 3i-k also demonstrated induction of apoptotic cell death of ovarian cancer (OVCAR-3, OVCAR-8) and colon cancer (HCT 116) cell lines and affected ERK signaling. In summary, 2-quinolyl-1,3-tropolones are promising compounds for development of effective anticancer agents.
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In this study, Gold-microrods (AuMRs), Pd-nanoparticles (PdNPs), and Polyaniline (PANI) nanocomposite-interface was fabricated on the screen-printed carbon-microelectrode (SPE). Each layer of the interface was characterised using field emission-scanning electron microscopy (FE-SEM) and cyclic voltammetry (CV). The fabricated SPE/AuMRs/PdNPs/PANI interface demonstrated the highest electronic current and showed excellent peroxidase-mimic towards H2O2 using chronoamperometry (CA). Furthermore, the SPE/AuMRs/PdNPs/PANI interface was utilised for the construction of a highly sensitive label-free electrochemical biosensor for the detection of Tpm in seafood samples. Label-free electrochemical detection of the Tpm was performed using both CA and differential pulse voltammetry (DPV) techniques. Preliminary data showed that both methods could detect Tpm as low as 0.01 pg/mL. Moreover, the developed biosensor for the detection of Tpm demonstrated excellent selectivity, high reproducibility and longer stability with an evident potential to detect Tpm in real seafood samples.
Assuntos
Compostos de Anilina , Técnicas Biossensoriais , Ouro , Chumbo , Nanopartículas Metálicas , Peroxidase , Tropomiosina , Compostos de Anilina/química , Biocatálise , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Microeletrodos , Peroxidase/química , Reprodutibilidade dos Testes , Tropomiosina/sangue , Tropomiosina/metabolismoRESUMO
Spinel NiCo2X4 (X = O or S), comprising two geometrical cobalt ions, Co2+ in the tetrahedral site (Co2+Td) and Co3+ in the octahedral site (Co3+Oh), has been widely evaluated as a promising pseudocapacitor electrode material. Previous literature mainly demonstrated that much higher specific capacitance of NiCo2S4 than that of NiCo2O4 was ascribed to the higher electronic conductivity. However, we argue that only a small amount of capacitance can be induced by the electronic conductivity, while the significance of electrochemical active species in these system has long been ignored. Here, we propose that geometrical-site-dependent pseudocapacitive activity will generate enhanced specific capacitance through the interface structural design. It reveals that specific capacitance of NiCo2S4 (1862 F g-1 at 4 A g-1) is 50% higher than that of NiCo2O4 (1230 F g-1 at 4 A g-1), which is derived from the designed increase of Co2+Td ions (cobalt ions in the tetrahedral site) in NiCo2S4. These results have significant implications for the design and optimization of the electrochemical properties of transition-metal-based pseudocapacitors.
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The development of low cost, portable diagnostic tools for in-field detection of viruses and other pathogenic microorganisms is in great demand but remains challenging. In this study, a novel approach based on reduced graphene oxide-polyaniline (rGO-PANi) film for the in situ detection of loop-mediated-isothermal-amplification (LAMP) products by means of open circuit potential measurement is proposed. The pH-sensitive conducting polymer PANi was electro-deposited onto rGO coated screen printed electrodes and tuned to be at the emeraldine state at which the pH sensitivity was maximized. By combining PANi and rGO, the pH sensitivity of the system was modulated up to about -64 mV per pH unit. This enabled the number of amplified amplicons resulting from the isothermal amplification process to be monitored. The sensor was then examined for monitoring LAMP reactions using Hepatitis B virus (HBV) as a model. This simple, low-cost, reproducible and sensitive interfacing layer is expected to provide a new possibility for designing point-of-care sensors under limited-resource conditions.
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Magnesium oxide (MgO) has been known as an excellent adsorbent for a variety of the environmentally polluted compounds. This work describes a synthesis of nanostructured MgO particles via a facile procedure by using cetyltrimethylammonium bromide (CTAB). Powder X-ray diffraction, thermal gravimetric, and differential thermal gravimetry (TGA/DTG) analyses were performed to characterize the physical properties of synthesized MgO particles and field emission-scanning electron microscopy (FE-SEM) was used to observe their morphology, whereas nitrogen adsorption-desorption isotherms and Brunauer-Emmett-Teller (BET) method were used to calculate the total surface areas of the samples. The adsorptive performance was studied by batch experiments for reactive blue (RB) 19 dye removal. The results showed that as-prepared MgO particles revealed hexagonal-like shaped platelets with an average diameter in the range of 49-91 nm and a mean thickness of 19-25 nm; meanwhile, MgO CTAB-free particles are aggregated, tiny nanoparticles with an average width of 22 nm and an average length of 77 nm. The maximum adsorption capacity of as-prepared nanostructured MgO for reactive blue (RB) 19 dye was 250 mg g(-1). Furthermore, the correlation between structural characterization (mean size, pore, surface) of the samples and the adsorption performance was also discussed in details.
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Antraquinonas/química , Óxido de Magnésio/química , Nanopartículas/química , AdsorçãoRESUMO
Comparison was observed for degradation and mineralization of the explosive 2,4,6-trinitroresorcine (TNR) in different photochemical systems TNR/UV, TNR/UV/TiO2, TNR/UV/H2O2, TNR/UV/O3, TNR/UV/TiO2/H2O2 and TNR/UV/TiO2/O3 using High Performance Liquid Chromatography coupled with Mass Spectrometry (HPLC/MS) and Total Organic Carbon (TOC) analysis. Addition of oxidizing agents such as H2O2 or O3 accelerated the rate of TNR conversion and mineralization. Highest reaction rate was obtained in TNR/UV/TiO2/H2O2 system. The intermediate products were characterized and identified by LS-MS technique. The similarity in intermediate products of TNR suggested the analogous reaction pathways of the TNR degradation by these different systems.
Assuntos
Minerais/química , Fotoquímica , Picratos/química , Picratos/efeitos da radiação , Resorcinóis/química , Resorcinóis/efeitos da radiação , Catálise/efeitos da radiação , Cromatografia Líquida de Alta Pressão , Peróxido de Hidrogênio/química , Concentração de Íons de Hidrogênio/efeitos da radiação , Espectrometria de Massas , Oxigênio/química , Soluções , Fatores de Tempo , Titânio/química , Raios Ultravioleta , Água/químicaRESUMO
Hydroxyapatite (HAp) coatings were prepared on 316L stainless steel (316LSS) substrates by electrochemical deposition in the solutions containing Ca(NO3)2·4H2O and NH4H2PO4 at different electrolyte concentrations. Along with the effect of precursor concentration, the influence of temperature and H2O2 content on the morphology, structure and composition of the coating was thoroughly discussed with the help of X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectra. The in vitro tests in simulated body fluids (SBF) were carried out and then the morphological and structural changes were estimated by SEM and electrochemical techniques (open circuit potential, polarization curves, Nyquist and Bode spectra measurements). Being simple and cost-effective, this method is advantageous for producing HAp implant materials with good properties/characteristics, aiming towards in vivo biomedical applications.
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Materiais Revestidos Biocompatíveis/química , Durapatita/química , Galvanoplastia/métodos , Aço Inoxidável/química , Eletricidade , Eletrodos , Eletrólitos/química , Peróxido de Hidrogênio/química , Microscopia Eletrônica de Varredura , Peso Molecular , Soluções , Espectrometria por Raios X , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura , Fatores de Tempo , Difração de Raios XRESUMO
A simple method was introduced to prepare magnetic chitosan nanoparticles by co-precipitation via epichlorohydrin cross-linking reaction. The average size of magnetic chitosan nanoparticles is estimated at ca. 30 nm. It was found that the adsorption of Cr(VI) was highly pH-dependent and its kinetics follows the pseudo-second-order model. Maximum adsorption capacity (at pH 3, room temperature) was calculated as 55.80 mg·g(-1), according to Langmuir isotherm model. The nanoparticles were thoroughly characterized before and after Cr(VI) adsorption. From this result, it can be suggested that magnetic chitosan nanoparticles could serve as a promising adsorbent for Cr(VI) in wastewater treatment technology.
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Quitosana/química , Cromo/isolamento & purificação , Fenômenos Magnéticos , Nanopartículas/química , Poluentes Químicos da Água/isolamento & purificação , Adsorção , Concentração de Íons de Hidrogênio , Cinética , Nanopartículas/ultraestrutura , Soluções , Temperatura , Fatores de Tempo , Difração de Raios XRESUMO
In spite of the technical important of monitoring CO(2) gas by using a semiconductor-type gas sensor, a good sensitive and selective semiconductor CO(2) sensor has been not realized due to the rather unreactive toward CO(2) of conventional semiconductor metal oxides. In this work, a novel semiconductor CO(2) sensor was developed by functionalizing SnO(2) nanowires (NWs) with LaOCl, which was obtained by heat-treating the SnO(2) NWs coating with LaCl(3) aqueous solution at a temperature range of 500-700°C. The bare SnO(2) NWs and LaOCl-SnO(2) NWs sensors were characterized with CO(2) (250-4,000 ppm) and interference gases (100 ppm CO, 100 ppm H(2), 250 ppm LPG, 10 ppm NO(2) and 20 ppm NH(3)) at different operating temperatures for comparison. The SnO(2) NWs sensors functionalized with different concentrations of LaCl(3) solution were also examined to find optimized values. Comparative gas sensing results reveal that LaOCl-SnO(2) NWs sensors exhibit much higher response, shorter response-recovery and better selectivity in detecting CO(2) gas at 400°C operating temperature than the bare SnO(2) NWs sensors. This finding indicates that the functionalizing with LaOCl greatly improves the CO(2) response of SnO(2) NWs-based sensor, which is attributed to (i) p-n junction formation of LaOCl (p-type) and SnO(2) nanowires (n-type) that led to the extension of electron depletion and (ii) the favorable catalytic effect of LaOCl to CO(2) gas.
Assuntos
Ar/análise , Dióxido de Carbono/análise , Ácido Hipocloroso/química , Lantânio/química , Nanofios/química , Compostos de Estanho/química , Catálise , Gases , Temperatura Alta , Semicondutores , Sensibilidade e EspecificidadeRESUMO
A voltammetric method based on a combination of incorporated Nafion, single-walled carbon nanotubes and poly(3-methylthiophene) film-modified glassy carbon electrode (NF/SWCNT/PMT/GCE) has been successfully developed for selective determination of dopamine (DA) in the ternary mixture of dopamine, ascorbic acid (AA) and uric acid (UA) in 0.1M phosphate buffer solution (PBS) pH 4. It was shown that to detect DA from binary DA-AA mixture, the use of NF/PMT/GCE was sufficient, but to detect DA from ternary DA-AA-UA mixture NF/SWCNT/PMT/GCE was required. The later modified electrode exhibits superior electrocatalytic activity towards AA, DA and UA thanks to synergic effect of NF/SWCNT (combining unique properties of SWCNT such as high specific surface area, electrocatalytic and adsorptive properties, with the cation selectivity of NF). On the surface of NF/SWCNT/PMT/GCE AA, DA, UA were oxidized respectively at distinguishable potentials of 0.15, 0.37 and 0.53 V (vs. Ag/AgCl), to form well-defined and sharp peaks, making possible simultaneous determination of each compound. Also, it has several advantages, such as simple preparation method, high sensitivity, low detection limit and excellent reproducibility. Thus, the proposed NF/SWCNT/PMT/GCE could be advantageously employed for the determination of DA in real pharmaceutical formulations.