Resumo em Inglês:

Low field time-domain nuclear magnetic resonance (TD-NMR) relaxometry of paramagnetic metal cations (PMC) has been widely used to study and improve contrast agents for magnetic resonance imaging (MRI). However, despite its remarkable potential, TD-NMR is rarely used to study PMC complexes, and coordination compounds in non-biomedical application. Therefore, this review aimed to provide comprehensive information not only to non-nuclear magnetic resonance (NMR) relaxation specialists, but also to scientists from distinct levels and expertise, as a way to pave the path for modern analytical and research of PMC complexes. Some fundamental concepts about NMR, paramagnetic relaxation mechanism, as well as traditional and modern methods to measure the longitudinal (T1) and transverse (T2) relaxation times constants are addressed. Here, we address some applications in analytical, electrochemical, and inorganic chemistry, electrodeposition reactions, as well as studies on PMC complexes and coordination compounds in solution.

Resumo em Inglês:

A fast, sensitive, and selective direct injection electrospray tandem mass spectrometry (DI ESI MS/MS) method that is able to quantify ethyl carbamate in commercial sweetened sugar cane spirit is described. The preparation method uses a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) with potassium carbonate added to sweetened sugar cane spirit to separate the aqueous phase from the ethanol phase. The aqueous phase contains sucrose that suppresses electrospray ionization. Ethyl carbamate supernatant from the ethanol phase is transferred and enriched with 18-crown-6/trifluoroacetic acid additives. The additives sequester metal cations reducing the ionization of sodium and potassium, favoring the detection of ethyl carbamate as sole protonated cations. The method was successfully applied for the quantification of eleven real samples and certified sugar cane spirit demonstrating its applicability for quality control and regulatory analysis. The method showed reliable analytical parameters compared to conventional gas chromatography mass spectrometry (GC-MS) method commonly used for ethyl carbamate analysis. DI-ESI-MS/MS method requires just a fast step sample clean up and presents consistent values for the limit of detection (LOD 48.0 μg L-1) and limit of quantification (LOQ 160.0 μg L-1). Furthermore, the recoveries obtained were close to 100%, with relative standard deviations below 10% of sample certificates.

Resumo em Inglês:

Glycerol can be determined in several products by various analytical techniques. Titrimetric ones have stood out for their low cost, being recommended as standards. However, reliable, simple, fast, and green methods with low quantification limits are still needed. Titration of glycerol is based on its oxidation by periodate (Malaprade reaction) producing formic acid, formic aldehyde, and iodate. Iodate and periodate are iodometrically titrated, but mutual interference between these ions has produced methods with some drawbacks. Here is proposed to mask periodate with molybdate, to eliminate interference, determining the glycerol content through iodate, employing iodometric titration. Solutions containing from 10 to 1000 µg of glycerol were analyzed (error < 3.4%). The method was successfully applied for the determination of glycerol in biodiesels from different raw materials. Recoveries were from 92.9 ± 0.4 to 111 ± 3%. Semi-micro extraction was done, providing a fast procedure for determining free glycerol in biodiesel (< 10 min).

Resumo em Inglês:

In this study, a laccaic acid-modified TiO2 photocatalyst (Lac-TiO2) was prepared via an impregnation method with 0.50, 1.00, 2.50, and 5.00 wt.% laccaic acid. The products’ physical properties were examined through X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), X-ray photoemission spectroscopy (XPS), UV-Vis diffused reflectance spectroscopy (DRS), Fourier-transform infrared spectroscopy (FTIR), nitrogen adsorption/desorption, and photoluminescence (PL) spectroscopy. A possible photocatalytic mechanism was also proposed. XRD patterns revealed the anatase phase of TiO2 and Lac-TiO2 samples. High-magnification FE-SEM images showed that the TiO2 and Lac-TiO2 samples exhibited spherical-like structures. XPS results complementarily confirmed the presence of Ti, O, and C as the main elements of the Lac-TiO2 samples. Interestingly, the DRS spectra of the Lac-TiO2 samples extended into the visible region. FTIR spectra presented the characteristic bands of TiO2 and hydroxyl groups on the TiO2 surface. Instead of hydroxyl groups, the characteristic bands of laccaic acid were observed on the surface of the Lac-TiO2 samples. The photocatalytic properties of the Lac-TiO2 samples were evaluated in terms of methyl orange degradation under visible light irradiation. The Lac-TiO2 samples showed higher photocatalytic performance than the TiO2 sample.

Resumo em Inglês:

According to the waste-to-energy (WTE) valorization and circular economy principles, the use of waste oil and grease (WOG) for obtaining biofuels shows the tendency towards sustainability, makes the interest in green chemistry, and the development of environmentally friendly processes grow. Three different fatty wastes (from the fat trap of a sewage station, lard waste, and frying oil) were analyzed and this work showed they have no potentially toxic metals. The frying oil sample and residual lard waste showed a higher percentage of triacylglycerides resulting in higher biodiesel conversion. The samples showed physical and chemical properties (density, viscosity, and ash) within the limits established by current regulations. Bio-oil samples formed a mixture of carboxylic acids, with high acidity. However, the parameters that deviated from the maximum permitted by the standard could be adjusted blending with petroleum diesel, replacing partially the fossil energy carriers with biomass-derived energy carriers which could bring positive impacts from multiple perspectives, i.e., economic, environmental, and health.

Resumo em Inglês:

Chikungunya virus (CHIKV) is a re-emerging disease caused by an alphavirus of the Togaviridae family. Since its first description in 1952, the disease has spread worldwide, affecting populations in both tropical and temperate countries. To date, there is no licensed vaccine or specific pharmacological treatment. Therefore, there is an increasing urgency in developing new antiviral drugs capable of specifically inhibiting viral replication. In the present work, we report the synthesis and antiviral activity evaluation of nineteen naphthoquinone derivatives, containing a sulfonamide or sulfonate group. Cell viability assays indicated a low toxic potential for all tested compounds and inhibitory assays against CHIKV identified five compounds with potent activity. The compounds were also evaluated for their virucidal potential, and the results demonstrated that compound 11a exhibited a virucidal effect higher than 70% in the treatment with 20 µM. Furthermore, in silico studies were performed to predict the antiviral drug targets.

Resumo em Inglês:

Water-soluble organic carbon (WSOC) makes up a large mass fraction of the organic carbon in the aerosol and can influence important cloud processes in the atmosphere. The capacity of WSOC to form metallic complexes with transition metals is well known; however, its influence on the aerosol of urban areas in the Amazon region is not very well known. In this study, we investigated the relationship between WSOC, black carbon (BC), levoglucosan (LEV) and transition metals (Fe, Cu and Mn) present in the PM2.5 (particles with a diameter smaller than 2.5 µm) of an urban environment during the dry season in the central Amazon. Oxalic acid (C2) was used to identify the influence of transition metals on WSOC. The mean mass concentration value of the PM2.5 was 14.72 μg m-3 (2.11-31.68 μg m-3). The WSOC made up 58.34% of the PM2.5 mass, followed by BC (20.28%), and LEV (2.62%). The WSOC showed significant correlation with the transition metals analyzed (> 0.56), especially Mn with C2 (linear coefficient (R2) = 0.74). A multiple linear regression with WSOC, BC and LEV showed a strong linear correlation between them (R2 = 0.86), indicating the influence of biomass burning and vehicle traffic on the organic aerosol.

Resumo em Inglês:

Citrus sudden death (CSD) is a disease that has affected millions of orange trees in Brazil, leading to economic losses in the order of billions of US dollars. This article examines the effects of CSD on the fatty acid composition of triacylglycerides (TAG) extracted from rootstock and scion bark. The fatty acid profile determined by gas chromatography showed a reduction in oleic and linolenic acids, and an increase in the saturated fatty acids and linoleic acid content, which was in line with the severity of CSD. The reduction in linolenic acid content was related to its role in the biosynthesis of jasmonic acid, which is involved in responses to abiotic and biotic stresses, as well as senescence. These alterations in the fatty acid profile were also used to classify plants both with and without CSD symptoms by using chemometric means. This method represents an alternative to support the diagnosis of CSD disease.

Resumo em Inglês:

In this work, two catalysts, lanthanum manganite strontium-doped perovskite without (LSM) and with (LSMMO) mixed molybdenum oxides, were synthesized by the sol-gel route and deposited by immersion in carbon cloth substrates. Their performance as cathodes in the hydrogen peroxide reduction reaction (HPRR) and oxygen reduction reaction (ORR) was investigated through cyclic voltammetry and electrochemical impedance spectroscopy, the electrocatalytic efficiency of these electrodes in the HPRR was analyzed in KOH and H2O2 medium at 298 K. The performance of the cathodes, in a single compartment, using a nickel plate as an anode was also investigated. The results showed that for the reduction reactions, electrodes developed with LSMMO have more significant catalytic activity than LSM after polarization, resulting in 32% higher current densities, lower electrical resistance after polarization, and a 21% increase in power density.

Resumo em Inglês:

In this paper, a pre-treatment process for electroless copper (Cu) deposition on the polished alumina (Al2O3) 99.9% and the behavior of Cu plating by electroless process after Al2O3 surface treatment were explored. Our work was carried out by changing the roughness of Al2O3 through micro-etching (coarsening), nucleation its surface by a two-step method (sensitization and activation) and electroless Cu plating deposited using non-commercial solution having formaldehyde as reducer, alkaline pH and operating temperature of 30 ºC. Contact angle system (CA), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), mechanical profilometer (DekTak XT) atomic force microscopy (AFM) and analysis by Gwyddion v2.27 software were used to evaluate the wet treatment and the morphology of the electroless deposition (ED) of Cu on the Al2O3 surface. The results show that the surface treatment of purity polished Al2O3 with 0.1% of vitreous materials present into the substrate surface, presents a high performance in ED film at low temperature (30 ºC), during the Cu deposition, obtaining more compact and uniform film, with small grain size, uniform thickness, and a high purity Cu metallic deposit.