The experimental activities for undergraduate chemistry students play an important role to develop skills and expertise in that science thus, the practice-experimental classes are so important to achieve this purpose. This work deals with a demonstrative experience for dye separation from food coloring sample using liquid column chromatography. Beyond the experimental practice and the facility in visualizing the separation, this demonstration shows how a simple experiment involving alternative and easy access materials can promote a meaningful learning once it is possible to handle the acquired data, trace and analyze the results themselves, thus developing skills rather than the operational procedure. This proposal could be implemented in initial chemistry classes in Brazilian universities. Sea and river sands were used as stationary phases and aqueous ethanolic solutions were used as mobile phases. A food coloring (a mixture of 3 dyes) was chosen as sample to be studied. Chromatographic separation was followed by spectrophotometric measurements. A set of analyses were carried out to discuss the solubility of the food coloring, granulometric studies of the stationary phases used and electronic microscopy images of the sands studied here. As alternative materials were used in this work, a chromatographic column was also constructed with low-cost materials.

This study evaluates the influence of milling on the reactivity of drilling cuttings (DC) utilized as supplementary cementitious material in ternary cements (TC). The drilling cuttings milling study varied the time (2, 5, 10, 15, and 20 min) and rotation speed (200 and 300 rpm), determining the specific milling energy and grindability index. The hydration of TC pastes containing DC with different particle size distributions was evaluated by isothermal calorimetry during the first 72 hours, XRD/Rietveld at 3 and 28 days, compressive strength and absorption. The incorporation of milled DC improved the TC hydration kinetics compared to reference pastes of ordinary Portland cement (REF.PC). After 28 days, the TC pastes with the D50% diameter smaller than 11 µm reached at least 70% of the resistance to the strength of the Portland cement paste. Milled DC contributes to the physical and nucleation effect of the TC pastes studied and can be used as an SCM.

RESUMO O catalisador residual (CR), oriundo do Craqueamento Catalítico Fluido (FCC) em refinarias de petróleo, tem sido estudado como pozolana em materiais cimentícios para avaliação do desenvolvimento de propriedades mecânicas e durabilidade. Contudo, estudos sobre a degradação destes materiais com dióxido de carbono supercrítico (scCO2) são recentes. Este artigo avalia a degradação de pastas endurecidas com substituição da massa do cimento por CR (0%, 15% e 30% de CR) expostas durante 7 h ao scCO2, na condição de temperatura e pressão estimada para 760 m de profundidade (53,55 °C/12,41 MPa). A densidade das pastas foi fixada em 1,89 g/cm3 e tempo de cura de 28 dias. A formulação das pastas e condição supercrítica visou simular a aplicação na estrutura de um poço onshore no nordeste do Brasil, considerando que o contato com scCO2 aconteça após ao enrijecimento das pastas. A microestrutura foi avaliada por Difratometria de Raios-X (DRX) e Análises Térmicas (TG/DTG e DTA), a rigidez mensurada por dureza superficial Rockwell (HR15T) e áreas carbonatadas calculadas após aspersão da solução indicadora de pH. As pastas com CR possuíram dureza superficial reduzida e maior teor de água livre, indicando maior porosidade em relação a pastas contendo somente cimento. As reações pozolânicas do CR causaram redução parcial do teor de hidróxido de cálcio [Ca(OH)2] e formação de compostos cimentícios [C-S-H, C-A-S-H, C-A-H e Af(t)]. Após a exposição ao scCO2, as pastas com CR possuíram área/profundidade de carbonatação maiores em relação à pasta 0% CR. A formação do CaCO3 acarretou acréscimo da dureza superficial principalmente nas pastas com CR. Devido as reações com scCO2, as pastas contendo CR tiveram compostos cimentícios parcialmente descalcificados, contudo, permanecendo com teores equivalentes ou superiores aos encontrados na pasta 0% CR cuja carbonatação causou redução parcial do Ca(OH)2.

ABSTRACT The residual catalyst (CR) from Fluid Catalytic Cracking (FCC) in petroleum refineries has been studied as pozzolan in cementitious materials to evaluate the development of mechanical properties and durability. However, studies on the degradation of these materials with supercritical carbon dioxide (scCO2) are recent. This article evaluates the degradation of hardened pastes with replacement of cement mass by CR (0%, 15% and 30% CR) exposed for 7 h to scCO2, in the temperature and pressure condition estimated at 760 m depth (53,55 °C / 12,41 MPa). The density of the slurries was set at 1.89 g/cm3 and curing time of 28 days. The formulation of the slurries and supercritical condition aimed to simulate the application in the structure of an onshore well in the northeast of Brazil, considering that the contact with scCO2 happens after the hardening of the slurries. The microstructure was evaluated by X-ray diffraction (XRD) and Thermal Analysis (TG / DTG and DTA), hardness measured by Rockwell surface hardness (HR15T) and carbonated areas calculated after the pH indicator solution was sprayed. The slurries containing CR had reduced surface hardness and higher free water content, indicating a higher porosity in relation to pure cement slurries. The pozzolanic reactions of CR caused partial reduction of calcium hydroxide [Ca(OH)2] content and formation of cementitious compounds [C-S-H, C-A-S-H, C-A-H and Af(t)]. After exposure to scCO2, the pastes with CR had a larger area/depth of carbonation than the 0% CR paste. The formation of CaCO3 resulted in an increase in surface hardness mainly in the pastes with CR. Due to the reactions with scCO2, the CR-containing pastes had partially decalcified cementitious compounds but remained equivalent to or higher than those found in the 0% CR paste whose carbonatation caused a partial reduction of Ca(OH)2.

Resumo O craqueamento catalítico em leito fluidizado (FCC) é usado para melhorar a eficiência do refino de petróleo e o resíduo catalítico gerado é denominado como “catalisador de equilíbrio” (Ecat). O seu uso em matrizes cimentícias vem sendo estudado por diversos laboratórios de pesquisas internacionais, avaliando a sua influência na pozolanicidade, comportamento mecânico, formação de produtos hidratados e durabilidade. Entretanto, sua influência na reologia de pastas de cimento ainda é pouco conhecida. Neste trabalho foi avaliada a influência do Ecat no comportamento reológico de pastas de cimento utilizando teores de substituição do cimento pelo resíduo em 10%, 20%, 30% e 40% em massa. Foram avaliados o tempo de pega e o comportamento reológico ao longo do tempo por meio dos ensaios de mesa de consistência, squeezeflow e reometria rotacional. Os resultados mostraram que o uso do Ecat influenciou no tempo de pega e no comportamento reológico das pastas estudadas. O módulo de fluidez proposto para o ensaio de squeezeflow se mostrou eficiente na análise do comportamento reológico das pastas estudadas.

Abstract Fluid bed catalytic cracking (FCC) is used to improve the efficiency of petroleum refining and the exhausted catalyst is referred to as "equilibrium catalyst", Ecat. The use of this catalytic residue in cementitious matrices has been studied by various international research laboratories, seeking to assess its influence on pozzolanicity, mechanical behavior, formation of hydrated products and durability. However, the influence of Ecat replacements on the Rheological behavior of cement pastes is not yet fully understood. Hence, this study evaluated the rheological properties of cement pastes with 10%, 20%, 30% and 40% by weight cement replacements. Setting time and time-dependent rheological behavior were investigated using consistency tests, squeeze flow and rotational rheometry. The results showed that the use of Ecat influenced the setting time and the rheological behavior of the pastes. The flow module proposed for the squeeze flow test was effective in analyzing the rheological behavior of the studied pastes.

Activated carbons (ACs) with well–developed microstructure and high microporosity were obtained from biomass by potassium hydroxide activation. The preparation process consisted in producing carbon materials in the ratios of activating agent to raw material 70:30, 50:50, 30:70 and 25:75 (w/w) characterized by thermal analysis coupled to spectroscopy (TG–DTA / FT–IR), scanning electron microscopy (SEM), N2 adsorption isotherms at –196 ºC and activation isotherm at 500 and 600 ºC for 3.0 h. Specific surface areas (SBET) within 728 and 1712 m2 g-1 and (Smic) within 1054 and 1923 m2 g-1 were obtained, while the micropores surface area was calculated using the Dubinin-Astakhov (DA) equation and the pore size distribution calculated from density functional theory (DFT) was found to be in the range 1.09 – 1.77 nm. Adsorption isotherms were fitted using Langmuir and Freundlich non–linear models and the adsorption capacity determined for methylene blue dye was between 27.13 and 459.20 mg g-1.

The reduction kinetics of a CuO/ZnO/Al2O3 catalyst by hydrogen was investigated isothermally and by temperature programmed reduction (TPR). Two reducible Cu2+ species were detected; the first one was identified as CuO bulk and the other as Cu2+ strongly interacting with alumina, possibly in the form of copper aluminate. The activation energies for the reduction of these two species were 60 and 90 kJ mol-1, respectively, and the reaction order with respect to hydrogen was one. The isothermal reduction data showed that the isotropic growth model is the most appropriate to describe the reaction rate data for both Cu2+ species.

The effect of operational variables and their interaction in TPR profiles was studied using a fractional factorial experimental design. The heating rate and the reducing agent concentration were found to be the most important variables determining the resolution and sensitivity of the technique. They showed opposite effects. Therefore, they should be manipulated preferentially in order to obtain optimized TPR profiles. The effect of sample particle size was also investigated. The tests were carried out within a Cu/Zn/Al2O3 catalyst used for the water-gas shift reaction that presented two distinct species of Cu2+ in TPR profiles.