Caracterização detalhada de material de referência certificado de carvão brasileiro

The use and characterization of the first Certified Reference Material (CRM) of Brazilian coal for analytical quality control are presented. All results were determined within the limits of repeatability and reproducibility allowed under the standards. Notable among the characterization parameters was the mineral matter content (45.39%) obtained by an alternative procedure showing a low relative error (-2.1%) compared to the standard technique (low ashing temperature). The possible expanded application of this CRM application in national laboratories, beyond the certificated and reference parameters, has advantages such as lower cost and easy availability, but round robin tests must be performed.

Análise exploratória rápida e não destrutiva (screening) da presença de elementos químicos tóxicos em material escolar por fluorescência de raios x

Compulsory in Brazil, toy certification aims to prevent possible risks in toy use. The Brazilian National Institute of Metrology (INMETRO) establishes the maximum concentration of toxic elements (TE) that may be present in toys. This study evaluates the presence of TE in different crayons, gouache and modeling clays using X-ray fluorescence. This technique is fast, has low operating cost and minimum sample pretreatment, resulting in a clean procedure without reagent consumption and waste generation. Bromine (in gouache) and Barium (in crayons) were the only potentially TE identified in the samples studied.

Síntesis química, estudios de caracterización y reactividad de un material catalítico a base de ZrO2-H3PW12O40

In this work, the preparation and characterization of materials such as zirconium oxide (ZrO2) and phosphotungstic acid promoted zirconium oxide (ZrO2-H3PW12O40) is presented. Physico-chemical characterization results showed that addition of H3PW12O40 acted as both a textural and chemical promoter of zirconium oxide. The incorporation of phosphotungstic acid into the ZrO2 matrix delayed the sintering of the material and stabilized ZrO2 in the tetragonal phase. ZrO2 acidity was also enhanced, developing strong acid sites on its surface. The Pt/ZrO2-H3PW12O40 catalyst was active for n-pentane isomerization at 250 °C, exhibiting high selectivity to iso-pentane (95%). This result is probably due to its suitable acidity.

Síntese do material mesoporoso MCM-41 usando esponja de água-doce como fonte de sílica

Fresh water sponge was used as a silica source for the synthesis of MCM-41 via the hydrothermal process. The silica was extracted from the sponge by washing with nitric acid and piranha solution. Synthesis of MCM-41 was performed at 100 °C for 5 days and the procedure was optimized, with modifications made to the leaching temperature of the silica and the synthesis of mesoporous material, which was characterized by XRD, FT-IR, SEM and adsorption of N2. The optimal result was achieved at a temperature of 135 °C for 3 days, showing ordered mesoporous material with a surface area of 1080 m² g-1.

Carboidratos como fonte de compostos para a indústria de química fina

Coal, oil, natural gas, and shale gas are biomass that is formed millions of years ago. These are non-renewable and depleting, even considering the recent discovery of new sources of oil in the presalt and new technologies for the exploitation of shale deposits. Currently, these raw materials are used as a source of energy production and are also important for the production of fine chemicals. Since these materials are finite and their (oil) price is increasing, it is clear that there will be a progressive increase in the chemical industry to use renewable raw materials as a source of energy, an inevitable necessity for humanity. The major challenge for the society in the twenty first century is to unite governments, universities, research centers, and corporations to jointly act in all areas of science with one goal of finding a solution to global problems, such as conversion of biomass into compounds for the fine chemical industry.Non-renewable raw materials are used in the preparation of fuels, chemical intermediates, and derivatives for the fine chemical industry. However, their stock in nature has a finite duration, and their price is high and will likely increase with their depletion. In this scenario, the alternative is to use renewable biomass as a replacement for petrochemicals in the production of fine chemicals. As the production of biomass-based carbohydrates is the most abundant in nature, it is judicious to develop technologies for the generation of chain products (fuels, chemical intermediates, and derivatives for the fine chemicals industry) using this raw material. This paper presents some aspects and opportunities in the area of carbohydrate chemistry toward the generation of compounds for the fine chemical industry.

Bateria de métricas para avaliação da verdura material de reações de síntese

The use of a battery of three mass metrics (atomic economy - AE, reaction mass efficiency - RME, and mass intensity - MI) for systemic evaluation of the material greenness of synthesis reactions is presented. Material greenness is discussed in terms of materialization/dematerialization of the reaction system and also according to the first two Principles of Green Chemistry, and is shown to involve two components: atomic greenness (incorporation of the atoms provided by reagents into the product, evaluated by AE and RME); and massic greenness (global mass of reagents and non-stoichiometric materials, evaluated by MI, related to the production of residues).

Theoretical investigations of the bulk modulus in the tetra-cubic transition of PbTiO3 material

Resulting from ion displacement in a solid under pressure, piezoelectricity is an electrical polarization that can be observed in perovskite-type electronic ceramics, such as PbTiO3, which present cubic and tetragonal symmetries at different pressures. The transition between these crystalline phases is determined theoretically through the bulk modulus from the relationship between material energy and volume. However, the change in the material molecular structure is responsible for the piezoelectric effect. In this study, density functional theory calculations using the Becke 3-Parameter-Lee-Yang-Parr hybrid functional were employed to investigate the structure and properties associated with the transition state of the tetragonal-cubic phase change in PbTiO3 material.

Dissulfeto de molibdênio, um material multifuncional e surpreendente: doze anos depois

In 2002, a review article was published in which molybdenum disulfide properties were discussed. The last sentence of the article read as follows: "Based on that described above, we can conclude that in spite of the vast applications of molybdenum disulfide in several industrial branches, many of the potential applications need to be investigated in the future". Since 2002, novel properties of molybdenum disulfide have been described which promise to revolutionize science. The objective of the present review paper was to provide an overview of the processes of 2H-MoS2 exfoliation and properties of the single layers, reported mainly in the last decade.

Sedimentação de nutrientes e material particulado em reservatório sob influência de atividades de piscicultura no semiárido do Rio Grande do Norte

Nutrient levels in water reservoirs have been increasing over the years worldwide and fish farming is one of the activities with the potential to cause negative impacts on these environments. Thus, the sedimentation of the main nutrients was evaluated in a reservoir as well as the contribution of aquaculture in raising these rates. The results indicated a significant difference for all nutrients, with higher concentrations in areas near the fish farming, and lower levels in more distant regions. Therefore, assessments that focus only on the water column do not reflect the true impact of this activity.

Potentiometric determination of Nickel (II) ion using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electroactive material

A potentiometric Nickel sensor was prepared using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electro-active material and epoxy resin as a binding material. A membrane composed of 40% Schiff's base and 60% epoxy resin exhibited the best performance. The membrane showed excellent response in the concentration range of 0.15 ppm to 0.1 mol L- 1 Ni+2 ions with non-Nernstian slope of 22.0 mV/decade, had a rapid response time (less than 10 s), and can be used for three months without any considerable loss of potential. The sensor was useful within the pH range of 1.3 to 9.6, and was able to discriminate between Ni2+ and a large number of alkaline earth and transition metal ions. The practical utility of the sensor has been demonstrated by using it successfully as an indicator electrode in the potentiometric titration of Ni2+ with EDTA and oxalic acid.

OBTENÇÃO E CARACTERIZAÇÃO DE MATERIAL HÍBRIDO ENTRE SÍLICA E CICLODEXTRINAS

The obtention of silica and cyclodextrin hybrid materials was accomplished by refluxing them in xylol using citric acid as a binding agent. The materials were characterized by infrared spectroscopy, X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, and elemental analysis. Evidence for the docking of cyclodextrins α and γ was substantiated based on the variation in band intensity for groups such as ≡Si-OH. Additional docking evidence includes the displacement of some of the bands that are related to cyclodextrin such as the deformation of the C-H axial bond. The α and γ-CDSi materials were characterized as amorphous compounds. The products obtained in the synthesis showed changes in the decomposition temperatures of their isolated constituents, in which the mass of α and γ-CD docked to the silica surface gave the estimated values of 41% and 47%, respectively. The elemental constituents were shown to be consistent and close to their relative theoretical values. ​Thermogravimetric analysis showed that a reduction in the percentage of the hybrids was proportional to the amount of lost mass. This new material is an improvement over synthesized organosilane materials because the operator and the environment benefit from a less toxic methodology. In addition, the material has several potential applications in complexation systems with cyclodextrin.

Desenvolvimento e aplicação de método GC-MS/MS para análise simultânea de 17 HPAs em material particulado atmosférico

Os hidrocarbonetos policíclicos aromáticos (HPAs) estão associados ao aumento da incidência de diversos tipos de cânceres no homem. Essas moléculas são formadas principalmente na queima incompleta de matéria orgânica, sendo encontradas em todos os compartimentos ambientais. Órgãos regulamentadores das áreas ambiental e de saúde ocupacional consideram 17 HPAs como contaminantes atmosféricos prioritários. Este trabalho apresenta um método para análise simultânea destes HPAs utilizando-se a cromatografia a gás acoplada à espectrometria de massas operando no modo tandem (GC-MS/MS). Os limites de detecção e quantificação do método mostraram-se até 5 vezes inferiores aos obtidos no método GC-MS (SCAN). O método mostrou-se seletivo para análise de HPAs em extratos de amostras de material particulado atmosférico. Uma análise comparativa de dois sistemas de solventes (diclorometano/metanol 4:1 v/v e hexano/acetona 1:1 v/v) para a extração de HPAs, utilizando amostras de material particulado atmosférico, revelou que ambas as misturas de solventes possuem poder de extração semelhante. Os resultados sugerem que é possível realizar extração de HPAs de material particulado atmosférico em ultra-som com a mistura hexano/acetona (1:1), que é menos tóxica em relação à mistura diclorometano/metanol (4:1), bastante utilizada nestas análises, sem perdas significativas na exatidão do método.

Aplicação de material zeolítico sintetizado de cinzas de carvão como adsorvente de poluentes em água

Cinzas leve de carvão tratadas pelo método hidrotérmico foram usadas como adsorvente de baixo custo para a remoção de íons metálicos e corante de solução aquosa. As isotermas de adsorção das cinzas leve tratadas foram estudadas e os resultados foram ajustados pelos modelos de Langmuir e Freundlich. A isoterma de Freundlich descreveu melhor o processo de adsorção do azul de metileno. Os dados de equilíbrio para a adsorção dos íons zinco e cádmio se ajustaram melhor á equação de Langmuir. O valor máximo de capacidade de adsorção obtido foi de 0,78 (mg g-1)(L mg)1/n para o azul de metileno, 38,1 mg g-1 para o Zn2+ e 67, 5 mg g-1 para o Cd2+. Os materiais sintetizados exibiram capacidades de adsorção muito maiores do que as das cinzas leves usadas como matéria-prima. O estudo mostrou que o material zeólitico pode efetivamente adsorver azul de metileno e íons metálicos com eficiências de remoção na faixa de 82-99%.

Uso de material didático sobre embriologia do sistema nervoso: avaliação dos estudantes

A Embriologia Humana é de extrema importância na formação de profissionais de saúde, porém seu estudo, muitas vezes, é considerado desestimulante, decorativo e sem significado prático para muitos estudantes, tornando-se pouco efetivo. Este trabalho objetivou produzir material didático interativo com modelos embrionários representativos do desenvolvimento embrionário do sistema nervoso. Para avaliar de forma qualitativa a real efetividade e capacidade de facilitar o processo de ensino-aprendizagem no contexto da Aprendizagem Baseada em Problemas, o material foi aplicado aos estudantes da primeira série de Medicina e Enfermagem da Faculdade de Medicina de Marília. Os estudantes consideraram que o material contribuiu para o entendimento do tema e facilitou a visualização dos eventos embrionários, além de despertar o interesse pelo estudo da disciplina. O material serviu como recurso para sedimentar o conhecimento e suscitou nos estudantes a integração dos conhecimentos com outras disciplinas. Em termos qualitativos, a análise dos questionários dos estudantes indicou que o material didático produzido foi efetivo na aprendizagem e funcionou como recurso na aprendizagem autodirigida, favorecendo a diversificação de fontes de busca e sendo complementar a livros-texto e outros materiais teóricos.

Inclusão de material herborizado em metacrilato para estudos de anatomia vegetal

As técnicas usuais empregadas no processamento de materiais herborizados são limitantes porque não permitem reproduzir um laminário permanente e porque o registro dos resultados é temporário. Em estudos de anatomia aplicada à taxonomia, muitas vezes, é necessário utilizar exsicatas. Este trabalho teve como objetivo testar a utilização de metacrilato (Historesin, Leica) na preparação e inclusão de material herborizado, visando a obtenção de laminário permanente. Foram utilizadas folhas de plantas herborizadas do gênero Senecio Tourn. ex L. (Asteraceae), previamente reidratadas em H2O e armazenadas em etanol 70%. As amostras foram desidratadas em série etanólica e submetidas à (1v:1v) mistura de AE 95% e resina pura. Durante a infiltração, com resina pura, o material foi submetido a vácuo durante 72 horas. Os blocos foram cortados em micrótomo de avanço automático, com navalhas de aço descartáveis, e os cortes foram corados com azul-de-toluidina (pH 4,0). As lâminas foram montadas em Permount. O laminário permanente obtido apresentou qualidade superior à dos produzidos pelas técnicas usuais, pois foi possível obter cortes seriados, com espessura determinada. Essa técnica possibilitou otimizar a obtenção de cortes, a partir de pequenos fragmentos de exsicatas.