Silver nanoparticles (AgNp) were deposited on highly porous TiO2 surfaces by the dripping of a colloidal AgNp solution to provide antimicrobial activity. Micro-porous TiO2 surfaces were obtained on commercially pure titanium by micro-arc oxidation in an electrolyte containing Ca and P precursors. In addition, as silver can be toxic to cells, these surfaces were uniformly covered with the biocompatible and bioresorbable poly(lactic acid) (PLA) polymer by electrospinning, aiming at promoting a controlled release of silver ions to the medium. The resulting AgNp-containing surfaces were characterized by scanning electron microscopy (SEM), energy dispersive spectrometry (EDS) and X-ray diffraction (XRD), and in vitro assays were performed to evaluate their antimicrobial activity and bioactivity. Tests revealed that the surfaces showed antimicrobial activity against Staphylococcus aureus, with better results for the surfaces without PLA. However, all the surfaces presented good biocompatibility in assays with mouse MC3T3-E1 pre-osteoblasts, and greater cell differentiation for the polymer-coated surfaces. Finally, the PLA ultrafine fibers electrospun on the TiO2/AgNp surfaces allowed a controlled release of silver ions in the phosphate-buffered saline (PBS) medium. (AgNp TiO Microporous Micro microarc micro arc precursors addition cells polylactic poly lactic acid (PLA electrospinning medium AgNpcontaining SEM, SEM , (SEM) EDS (EDS Xray X ray XRD, XRD (XRD) bioactivity aureus However MC3T3E1 MCTE MC3T3 E1 MC T E MC3T3-E preosteoblasts, preosteoblasts pre osteoblasts, osteoblasts pre-osteoblasts polymercoated coated Finally TiO2AgNp TiOAgNp phosphatebuffered phosphate buffered PBS (PBS (SEM (XRD MC3T3E MCT MC3T

Considering the bicentenary of Brazil’s Independence in 2022 and that this year was proclaimed by UNESCO as the International Year of Basic Sciences for Sustainable Development, in mid-2021 the Brazilian Chemical Society (SBQ) launched the “Post 2022 Chemistry Movement - Sustainability and Sovereignty”, with the main goal of promoting different activities so that chemistry contributes for the sustainable development and sovereignty of Brazil in the coming years. One of these activities is the proposal of an action plan, with goals to be achieved by 2030 and 2050. This article describes in detail how this action plan was formulated by a working group, with the help of an advisory council and interviews of 18 professionals from universities, the government, industries, the third sector and other organizations. Mimicking the Agenda 2030 SDGs, the resulting action plan is based on two broad Chemistry Sustainable Development Goals: promoting sustainability through chemistry in basic education, and promoting sustainability in the industry and university through science, technology, innovation, and education (STI&E) in chemistry. After the definition of three driving technological challenges in STI&E, they shall be successively implemented through different actions starting in 2023 yet.

Simple, fast, and inexpensive electroanalytical procedures were developed for the determination of codeine (COD) solely and paracetamol (PCT) and COD simultaneously in pharmaceutical formulations and human body fluids. The methods involve the combination of square-wave voltammetry (SWV) with a cathodically pretreated boron-doped diamond electrode and a 0.2 mol L–1 acetate buffer (pH 4.0) solution as the supporting electrolyte. Significantly low limits of detection were obtained for COD solely or PCT and COD simultaneously: 1.19 or 18 and 14 nmol L–1, respectively. The proposed SWV method was successfully applied in the simultaneous determination of PCT and COD in four samples of pharmaceutical tablets, with results similar (at 98% confidence level) to those obtained using a reference high-performance liquid chromatography (HPLC) method. Additionally, adequate results were obtained when concentrations of PCT and COD were determined in human urine or serum samples by addition-recovery. Clearly, the proposed method is an excellent option for the determination of COD solely or PCT and COD simultaneously.

The Direct Black 22 dye was electrooxidized at 30 mA cm-2 in a flow cell using a BDD or β-PbO2 anode, varying pH (3, 7, 11), temperature (10, 25, 45 °C), and [NaCl] (0 or 1.5 g L-1). In the presence of NaCl, decolorization rates were similar for all conditions investigated, but much higher than predicted through a theoretical model assuming mass-transport control; similar behavior was observed for COD removal (at pH 7, 25 °C), independently of the anode. With no NaCl, COD removals were also higher than predicted with a theoretical model, which suggests the existence of distinct dye degradation pathways.

Um procedimento simples é descrito para a determinação de propiltiouracil (PTU) por voltametria de pulso diferencial (DPV) usando um eletrodo de diamante dopado com boro (BDD) pré-tratado catodicamente. Estudos por voltametria cíclica indicam que a oxidação do PTU é irreversível a um potencial de pico de 1,42 V (vs. Ag/AgCl (KCl 3,0 mol L-1)) em uma solução tampão de Britton-Robinson (BR) (pH 2,0). Sob condições otimizadas, a curva analítica obtida foi linear (r = 0,9985) na faixa de concentração de PTU de 1,0 a 29,1 mmol L-1 em solução tampão BR (pH 2,0), com um limite de detecção de 0,90 mmol L-1. O método proposto foi aplicado com sucesso na determinação de PTU em amostras farmacêuticas, com resultados concordantes (a um nível de 95% de confiança) com aqueles obtidos empregando um método titulométrico oficial.

A simple procedure is described for the determination of propylthiouracil (PTU) by differential pulse voltammetry (DPV) using a cathodically pretreated boron-doped diamond (BDD) electrode. Cyclic voltammetry studies indicate that the oxidation of PTU is irreversible at a peak potential of 1.42 V (vs. Ag/AgCl (3.0 mol L-1 KCl)) in a Britton-Robinson (BR) buffer solution (pH 2.0). Under optimized conditions, the obtained analytical curve was linear (r = 0.9985) for the PTU concentration range of 1.0 to 29.1 mmol L-1 in a BR buffer solution (pH 2.0), with a detection limit of 0.90 mmol L-1. The proposed method was successfully applied in the determination of PTU in pharmaceutical samples, with results in agreement at a 95% confidence level with those obtained using an official titration method.

A remoção de íons Pb2+ a partir de soluções diluídas foi estudada, em condições galvanostáticas, usando uma célula de fluxo sem membrana com eletrodos de esponja de aço inoxidável (SSW). A metodologia de superfície de resposta (variáveis independentes: corrente elétrica e vazão) foi usada para obter as condições ótimas para a remoção de Pb2+ a partir de 2 L de uma solução de Pb(NO3)2 50 mg L-1 em NaNO3 0,10 mol L-1 + H3BO3 0,10 mol L-1 (pH 4,8). A partir das superfícies de respostas, concluiu-se que a vazão (59-341 L h-1) não influencia significativamente no processo de remoção de Pb2+. Por outro lado, o aumento da corrente elétrica leva a uma maior remoção de Pb2+, com valores significantemente melhores de consumo de energia específica e eficiência de corrente quando comparados àqueles relatados na literatura. Para um experimento realizado na região de condições ótimas (70 mA e 200 L h-1), uma conversão de Pb2+ de 99,6% foi atingida depois de 90 min de eletrólise. A utilização da célula de fluxo sem membrana com eletrodos de SSW, além de ser energeticamente mais eficiente, levou à remoção de Pb2+ em ambos os eletrodos, mais predominantemente no anodo, sobre o qual 95% dos íons Pb2+ foram convertidos a PbO2.

The removal of Pb2+ ions from dilute solutions was investigated under galvanostatic conditions using a membrane-less flow-through cell with stainless steel wool (SSW) electrodes. The response surface methodology (independent variables: electric current and volumetric flow rate) was used to find the optimal conditions for Pb2+ removal from 2 L of an aqueous solution of 50 mg L-1 Pb(NO3)2 in 0.10 mol L-1 NaNO3 + 0.10 mol L-1 H3BO3 (pH 4.8). The obtained response surfaces revealed that the volumetric flow rate (59-341 L h-1) does not substantially affect the Pb2+ removal process. On the other hand, the electric current increase led to higher Pb2+ removal, with significantly improved values of specific energy consumption and current efficiency when compared with those reported in the literature. For an experiment carried out in the optimum-condition region (70 mA and 200 L h-1), a Pb2+ conversion of 99.6% was attained after 90 min of electrolysis. The use of the membrane-less flow-through cell with SSW electrodes, besides being significantly more energy efficient, led to Pb2+ removal on both electrodes, but predominantly in the SSW anode, on which more than 95% of the Pb2+ ions were converted to PbO2.

A degradação eletroquímica do corante Vermelho Reativo 141 foi investigada por meio da aplicação da metodologia de superfície de respostas, utilizando reator filtro-prensa com anodo de β-PbO2. A carga requerida para 90% de descoloração (Q90) e a remoção da demanda química de oxigênio após 30 min de eletrólise (COD30) foram utilizadas para modelar o sistema. As variáveis investigadas foram a densidade de corrente, pH, concentração de NaCl e temperatura. Baixos valores de Q90 (0,2-0,3 A h L-1) foram obtidos em condições ácidas (pH 1-3) e em altas concentrações de NaCl (1,0-2,0 g L-1), quando as espécies oxidantes Cl2 e HOCl estão presentes. Os melhores valores para COD30 foram obtidos com altas densidades de corrente e em condições de pH ácido a neutro; entretanto, o consumo energético resultante torna o processo economicamente não viável. Para soluções extremamente ácidas foram obtidos valores reduzidos de consumo de energia, relacionado ao Q90, em torno de 0,79 kW h m-3.

The electrochemical degradation of the Reactive Red 141 dye using a filter-press reactor with a β-PbO2 anode was investigated through the application of the response surface methodology. The charge required for 90% decolorization (Q90) and the chemical oxygen demand removal percentage after 30 min electrolysis (COD30) were used to model the system. The investigated independent variables were the current density, pH, NaCl concentration, and temperature. Low values of Q90 (0.2-0.3 A h L-1) were obtained at acidic conditions (pH 1-3) and high concentrations of NaCl (1.0-2.0 g L-1), when Cl2 and HOCl are the predominant oxidant species. The best values of COD30 were obtained at high current densities and acidic to neutral conditions (pH 5-7); however, the consequent energy consumption makes the process not economically feasible under these conditions. For strongly acidic solutions, specific energy consumptions associated to Q90 as low as 0.79 kW h m-3 were attained.

The electrochemical performance of electrodeposited Ti/β-PbO2 and Ti-Pt/β-PbO2 anodes was galvanostatically evaluated (batch mode, 50 mA cm-2) to degrade the Direct Yellow 86 dye (100 or 200 mg L-1 in 0.1 mol L-1 Na2SO4 + 1.5 g L-1 NaCl), investigating the effect of pH and temperature. Similar results were obtained for both electrodes and the best conditions for removal of color and chemical oxygen demand are pH 7 and 40 °C, when 90% decolorization is attained by passing a charge of only ~0.13 A h L-1 and total mineralization is achieved with expenditure of ~5 kW h m-3.

Neste trabalho descreve-se a determinação do ácido acetilsalicílico (ASA) em formulações farmacêuticas empregando voltametria de onda quadrada (SWV) e um eletrodo de diamante dopado com boro (BDD). Neste método, ASA é determinado diretamente em solução de H2SO4 0,01 mol L-1, sem a necessidade da hidrólise alcalina. Foi obtido um único pico de oxidação no potencial de 1,97 V vs. Ag/AgCl (KCl 3,0 mol L-1) com características de uma reação irreversível. A curva analítica obtida é linear na faixa de concentração ASA de 2,50 × 10-6 -1,05 × 10-4 mol L-1, com um limite de detecção de 2,0 µmol L-1. O desvio padrão relativo foi menor que 1,4% para uma solução de ASA 45 µmol L-1 (n = 10). O método proposto foi aplicado com sucesso para a determinação de ASA em várias formulações farmacêuticas e os resultados obtidos foram concordantes com um método oficial da Farmacopéia Britânica, a um nível de confiança de 95%.

In this paper the determination of acetylsalicylic acid (ASA) in pharmaceutical formulations using square-wave voltammetry (SWV) and a boron-doped diamond electrode (BDD) is described. By this proposed method, ASA is directly determined in a 0.01 mol L-1 H2SO4 solution without the need of a previous time-consuming alkaline hydrolysis step. A single oxidation peak at a potential of 1.97 V vs. Ag/AgCl (3.0 mol L-1 KCl) with the characteristics of an irreversible reaction was obtained. The obtained analytical curve is linear in the ASA concentration range 2.50 × 10-6-1.05 × 10-4 mol L-1, with a detection limit of 2.0 µmol L-1. The obtained relative standard deviation was smaller than 1.4% for a 45 µmol L-1 ASA solution (n = 10). The proposed method was applied with success in the determination of ASA in several pharmaceutical formulations; the obtained results were in close agreement, at a 95% confidence level, with those obtained using an official method of the British Pharmacopoeia.

The use of square-wave voltammetry in conjunction with a cathodically pre-treated diamond electrode for the analytical determination of sodium cyclamate is described. The samples were analyzed as received in a 0.5 mol L-1 H2SO4 solution in the concentration range from 5.0 × 10-5 mol L-1 to 4.1 × 10-4 mol L-1, with a detection limit of 4.8 × 10-6 mol L-1. The RSD was smaller than 1.2 % and the proposed method was applied with success in the determination of sodium cyclamate in several dietary products.

This article offers an overview on the historical facts and the recent state of the Regional Secretaries and the Scientific Divisions in the course of 30 years of SBQ.

Descreve-se o desenvolvimento e validação de um método de CLAE para acompanhar a degradação de fenol por tratamento eletroquímico ou fotoeletroquímico. Este método, que permite a determinação das quantidades de fenol, p-benzoquinona e catecol em soluções eletrolisadas ou fotoeletrolisadas, foi usado para análise dos intermediários de reação durante a eletroxidação ou fotoeletroxidação de fenol. Foram usados como eletrodos, Ti-Pt/PbO2 (obtido por método térmico-eletroquímico ou por eletrodeposição) ou Ti/TiO2 dopado com Ga3+ (obtido por decomposição térmica de sais precursores).

The development and validation of a HPLC method to follow the degradation of phenol by electrochemical or photoelectrochemical treatment are described. This method, which allows determining amounts of phenol, p-benzoquinone and cathecol in electrolyzed or photoelectrolyzed solutions, was used for analysis of reaction intermediates during electrooxidation or photoelectrooxidation of phenol using a Ti-Pt/PbO2 (obtained by thermal-electrochemical or electrodeposition methods) or Ti/TiO2 doped with Ga3+ (obtained by thermal decomposition of precursor salts) electrode.

The physical and electrochemical properties of Ti-SnO2/Sb electrodes obtained by the thermal decomposition of solutions of the precursor salts SnCl2×2H2O/SbCl3 and SnSO4/Sb2(SO4)3 were investigated. The reversibility of the cyclic voltammetric response of the Fe(CN)6(4-)/Fe(CN)6(3-) redox couple was assessed using the obtained electrodes. Their catalytic activity for the oxygen-evolving reaction and maximum capacity for electronic transfer were also evaluated by potential and current linear scans in 0.5 mol L-1 H2SO4. Additionally, scanning electron microscopy analyses allowed the visualization of the morphology of the oxide films obtained. The best results were presented by the electrodes obtained from the chloride salt precursors.