The objectives of this study were twofold: to assess two chromatographic methods for the analysis of greenhouse gases (GHG) and carbon monoxide, and to propose and evaluate a low-cost and reusable alternative system for their sampling and storage, using 10 different container configurations (flasks and bags). To that end, standard samples containing the gases of interest (CO2, CH4 and CO) and different types of real samples were tested. Finally, procedures for the sampling, storage and analysis of CO2 and CH4 were evaluated and optimized. Two chromatographic methods were applied, using different analysis conditions and columns. Gas chromatography analysis of sample stability and container reusability demonstrated that borosilicate flasks with butyl rubber and PTFE/silicone septa are ideal for storing samples, allowing up to 5 successive sampling cycles with no significant loss of recovery. For larger volume samples, multilayer foil bags are the most stable for the compounds analyzed. The tests conducted with real and synthetic gas samples under optimized chromatography conditions using both methods indicated satisfactory performance for CO2 and CH4 quantification. However, CO analysis in the column with a polystyrene-divinylbenzene stationary phase (Method 1) produced an artifact due to the presence of oxygen in the samples, restricting its quantification.

We evaluated solid-state sensors (MOS) manufactured using nanostructured tin oxide (SnO2) obtained by different synthesis methods for selectivity, response and repeatability at different operating temperatures and methane concentrations. In addition, Zeolite 13X pellets were placed in front of the sensors to improve CH4 selectivity in the presence of CO2. The palladium doped sensor (1.4% w/w) showed the highest sensitivity at 80 ºC (83%) and shorter response times (16 s), whereas non-doped sensors exhibited the best sensitivity (78%) and response times (14 s) for those with smaller particle size (8 nm). Zeolite 13X pellets proved to be efficient at making the sensor more selective for CH4 in the presence of CO2.

Aluminium alloy Al-Si5Cu3 (319) is one of the most commonly used casting alloys for automobile components, due to its casting characteristics. Iron is the major impurity element that influences the detrimental β-phase formation in secondary aluminum alloys. In the present study, we investigated the influence of the cooling rate on the formation of iron compounds, α-Al15(Mn,Fe)3Si2 and β-Fe5AlSi phases, in Al-Si5Cu3 containing 1.0% Fe, 0.5% Mn and 0.2% Mg, by thermal analysis and metallography. The results show that the high cooling rates, between 10-103 K/s, are able to reduce and nullify the formation of needle-like β-Al5FeSi phase, and help the formation of the Chinese scripts α-Al15(Fe,Mn)3Si2 phase. The analysis of the curves reveals that the increase of the cooling rate increases the temperature of nucleation of the α-Al dendrite and decrease the eutectics Al-Si and Al-Cu phases.

Abstract The influence of tellurium in the indium segregation of Ga1-xInxSb:Te ingots obtained by the conventional vertical Bridgman method (CVBM), under stirred and non-stirred conditions, was investigated. Three Te-doped ingots and three no-doped ingots were unidirectionally solidified at a constant speed of 2.0 mm/hour, inside quartz ampoules, closed under argon, and with a conical tip. The furnace temperature was set for overheating between 73.5 - 93ºC, and temperature gradients between 3.0 - 3.3ºC/mm. The tellurium doped ingots showed a smaller number of grains and no cracks in the middle region of the ingots, right after the tip, in comparison with the no-doped ingots. Moreover, when comparing the stirred with the non-stirred ingots, the EDS experimental profile of indium in Te-doped synthetized without melt stirring ingot showed a better agreement with the Scheil-Gulliver equation than the stirred Te-doped ingots. The Te-doped ingots when stirring the melt during synthesis showed a more constant axial indium distribution, up to 85% of their lengths. The constant lattice estimated from TEM diffraction images are respectively 6.29 Å for the non-doped sample and 6.17 Å for the Te-doped sample. A qualitative account for the increase of the lattice parameter and the Hall measurements results is that the tellurium compensates for the native acceptor defects, contributing to the microstructural quality in the Ga1-xInxSb ingots.

Abstract The fit of the implant-abutment interface was assessed by the metallographic technique and by scanning electron microscopy (SEM), using solid abutment types at different torque levels. Forty Morse taper connections and forty solid abutments were used at different torque levels (repeated after 10 minutes) in the following groups (n = 10): 25 Ncm (group g1), 30 Ncm (group g2), 35 Ncm (group g3), and 40 Ncm (group g4). The samples were embedded in a metallographic resin, sectioned lengthwise, and polished. SEM images were used to measure the linear contacts and the fits between abutments and the internal walls of the implant. The overall mean gap and standard deviation were as follows: 9.0 ± 1.36 µm for group g1, 7.9 ± 2.81 µm for group g2, 2.0 ± 0.76 µm for group g3, and 0.3 ± 0.40 µm for group g4. A significant difference was observed in the average fit values between the groups (p < 0.05). The linear area of contact between the abutment and the implant increased as torque augmented. This study demonstrated that higher insertion torque values in a conical internal connection increase the fit (contact) of the implant-abutment interface.

The species and density of Eucalyptus wood poles installed in the electrical network are useful parameters which must be considered when it is necessary to establish the service life of these structures. In this work, eucalyptus poles samples were collected and analyzed by scanning electron microscopy and energy dispersive spectroscopy (SEM/EDS). SEM image analysis showed that the lumen diameter average of fiber substantially is variable between the three species studied, in line with the wood density obtained in laboratory, for poles with several years in service in the electricity network, as well as for not used poles. In addition, EDS microanalysis was utilized for identify the presence of chemical preservatives employed in the conservation these poles. The analysis method proposed proved effective for characterization for this timber.

Este trabalho apresenta correlações obtidas entre propriedades mecânicas, densidade e o estado de deterioração de postes de eucalipto novos e retirados de serviço. O estado de deterioração foi determinado por inspeções em campo de postes da rede de distribuição de energia elétrica no sul do Brasil. Postes em diferentes estados de deterioração foram retirados da rede para os ensaios de flexão estática e medidas de densidade. Os testes mecânicos indicaram que os valores médios da resistência a flexão e da rigidez decrescem com o estado de deterioração do eucalipto. Entretanto, verificou-se uma grande variação nessas medidas com diferentes classes de deterioração apresentando resistência mecânica residual similar. Esse comportamento pode ser explicado pela influência da densidade da madeira nas correlações entre propriedades mecânicas e o estado de deterioração dos postes. Madeiras menos densas podem apresentar baixa resistência mecânica residual mesmo sem apresentar sinais de deterioração. O estudo da caracterização da madeira de eucalipto indicou que o estado de deterioração avaliado pela inspeção em campo, por si só não é um bom indicativo para prever a durabilidade das estruturas de madeiras, fazendo-se necessária uma análise preliminar da densidade da mesma.

This paper presents the correlations obtained among mechanical properties, density and deterioration status of new eucalyptus poles and those removed from service. The deterioration status was determined in the field in sections of poles of the distribution of electric energy in southern Brazil. Poles in various status of deterioration were removed from the network for static bending tests and density measurements. The mechanical tests indicated that the average values of bending strength and stiffness decline with the deteriorating state of eucalyptus. However, there was a large variation in these measures with different classes of deterioration presenting similar residual mechanical strength. This behavior can be explained by the influence of wood density on the correlations between mechanical properties and the state of deterioration of the poles. Less dense woods can have residual mechanical strength low even without present signs of deterioration. The study of the characterization of eucalyptus wood indicated that the state of deterioration measured by field inspection alone is not a good indicator for predicting the durability of wood structures, making necessary a preliminary analysis of the density.

Consolidação por Constrição Radial (CCR) é uma técnica de metalurgia do pó que possibilita a obtenção de peças metálicas próximas da forma final, com alta densidade e de formas complexas, com custos de produção mais baixos que as tecnologias convencionais. CCR assemelha-se, em alguns aspectos, ao processo de compactação isostática a quente, sendo que as principais diferenças referem-se ao fato de que o processo CCR utiliza moldes cerâmicos fabricados a partir do processo de microfusão e usa um meio compressor secundário na forma de pó, ambos confinados em um container metálico. Nesse trabalho, desenvolveu-se um sistema experimental de CCR, visando à produção de pré-formas de ferro de alta densidade. Como meio compressor secundário, foi utilizado pó de argila calcinada. As pré-formas produzidas foram caracterizadas quanto à densidade, microestrutura e dureza. Observou-se que a configuração do container metálico/meio compressor secundário/molde cerâmico tem grande influência nas características de densidade e dimensionais das pré-formas. As pré-formas obtidas apresentaram consolidação satisfatória do pó como indicado pela microestrutura apresentada, alta densidade, elevada dureza, pouca formação de óxido e uma correlação direta entre os valores de dureza e densidade.

The Radial Constriction Consolidation (RCC) process can be considered a powder metallurgical technique that allows for the fabrication of components with complex geometries, near-net-shape and full density at low production costs when compared to the traditional process. In some aspects, the RCC process is similar to the hot isostatic pressing process, but it uses a ceramic mold confectioned by investment casting and a powder as a secondary pressing media, all of which are confined in a metallic container. In this paper, a RCC experimental system was developed aiming to produce iron billets with the characteristics of near-net-shape and high density. Clay powder was used as a secondary pressing media. The obtained billets were characterized in terms of density, microstructure and hardness. It was observed that the configuration of the metallic container/ secondary pressing media/ceramic mold has an important influence on the characteristic of density and near-netshape of the billets. The billets presented satisfactory powder consolidation as shown in their microstructure, high density, elevated hardness, little oxide formation and a direct correlation between the values of density and hardness.

OBJETIVO: analisar, por meio de microscopia eletrônica de varredura, as alterações químicas e estruturais de braquetes metálicos submetidos a um processo de biodegradação in vitro. MÉTODOS: a amostra foi dividida em dois grupos, de acordo com a marca comercial dos acessórios - Grupo A = Dyna-Lock, 3M/Unitek (AISI 303) e Grupo B = LG Edgewise Standard, American Orthodontics (AISI 316L). Os corpos de prova, aparelhos ortodônticos simulados, permaneceram imersos em solução salina (0,05%) por um período de 60 dias, a 37ºC, sob agitação. As alterações decorrentes da exposição dos acessórios à solução salina foram investigadas através da observação com microscópio eletrônico de varredura (MEV) e análise da composição química (EDX), realizadas antes e após o período de imersão (T0 e T5, respectivamente). RESULTADOS: em T5, houve formação de produtos de corrosão sobre a superfície dos braquetes, especialmente no Grupo A, além disso, houve alterações na composição da liga metálica dos braquetes de ambos os grupos, sendo que, no Grupo A, houve redução dos íons ferro e cromo e, no Grupo B, redução de íons cromo. CONCLUSÃO: os acessórios do Grupo A apresentaram-se menos resistentes à biodegradação in vitro, o que poderia estar associado ao tipo de aço utilizado em sua fabricação (AISI 303).

OBJECTIVES: The purpose of this study was to analyze, with the aid of scanning electron microscopy (SEM), the chemical and structural changes in metal brackets subjected to an in vitro biodegradation process. METHODS: The sample was divided into three groups according to brackets commercial brand names, i.e., Group A = Dyna-Lock, 3M/Unitek (AISI 303) and Group B = LG standard edgewise, American Orthodontics (AISI 316L). The specimens were simulated orthodontic appliances, which remained immersed in saline solution (0.05%) for a period of 60 days at 37°C under agitation. The changes resulting from exposure of the brackets to the saline solution were investigated by microscopic observation (SEM) and chemical composition analysis (EDX), performed before and after the immersion period (T0 and T5, respectively). RESULTS: The results showed, at T5, the formation of products of corrosion on the surface of the brackets, especially in Group A. In addition, there were changes in the composition of the bracket alloy in both groups, whereas in group A there was a reduction in iron and chromium ions, and in Group B a reduction in chromium ions. CONCLUSIONS: The brackets in Group A were less resistant to in vitro biodegradation, which might be associated with the type of steel used by the manufacturer (AISI 303).

A liga Zn-22%Al apresenta uma microestrutura complexa, tanto no estado bruto de fusão, como após envelhecimento, devido à transformação eutetóide (β → α + η). O objetivo desse trabalho é relacionar a morfologia das fases presentes em lingotes brutos de fusão e após envelhecimento com a taxa de solidificação. Amostras dos lingotes da liga Zn-22%Al foram analisadas por microscopia eletrônica de varredura (MEV) e EDS (Energy Dispersive Spectroscopy). A estrutura α + η com morfologia lamelar em amostras brutas de fusão transforma-se em uma textura refinada tendendo a globular-equiaxial após o envelhecimento. Observou-se que a dureza das amostras está fortemente relacionada com a morfologia da estrutura α + η. Por outro lado, a composição e a morfologia das fases são conseqüências da taxa de solidificação e resfriamento.

The Zn22wt%Al alloy has a complex microstructure due to eutectoid transformation (β → α + η) in cases of as-casting and after quench-aging conditions. The objective of this work was to investigate the relationship between the solidification rate and the morphology of α and η phases, before and after quench-aging. The samples of the Zn-22wt%Al alloy were analyzed by scanning electron microscopy (SEM) and by EDS (Energy Dispersive Spectroscopy). The as-casting samples presented a lamellar structure while the as-aged ones exhibited a quasi-globular morphology. The results showed that the hardness of the samples strongly depends on the α + η phase morphology. On the other side, the chemical composition and morphology of the phases depends on the solidification and cooling rates.

OBJETIVO: avaliar, in vitro, a biodegradação de aparelhos ortodônticos simulados constituídos de braquetes e fios de aço inoxidável. METODOLOGIA: a amostra foi dividida em 2 grupos, de acordo com a marca dos braquetes usados: grupo A - Dyna-Lock, 3M/Unitek (AISI 303); e grupo B - LG Edgewise Standard, American Orthodontics (AISI 316L). Os corpos-de-prova permaneceram incubados em solução salina (0,05%) a 36ºC, sob agitação por um período de até 60 dias. A análise da liberação iônica foi realizada por meio de espectrofotometria de absorção atômica. O peso em massa dos braquetes também foi medido antes e após o experimento. RESULTADOS: os resultados indicaram que o grupo A apresentou maior liberação de íons ferro, níquel e cromo do que o grupo B. Além disso, os braquetes do grupo A também mostraram perda de massa, considerada outro indicativo de corrosão. CONCLUSÃO: concluiu-se que, nas condições deste experimento, os braquetes do grupo A apresentaram maior biodegradação que os acessórios do grupo B, o que pode estar associado à liga metálica e/ou ao processo de fabricação dos mesmos.

OBJECTIVE: The purpose of this study was to evaluate, in vitro, the biodegradation of simulated orthodontic appliances consisting of stainless steel brackets and wires. MATERIALS AND METHODOS: The sample was divided in 2 groups, according to brackets brand: group A - Dyna-Lock, 3M/ Unitek (AISI 303); and group B - LG Edgewise Standard, American Orthodontics (AISI 316L). The specimens (simulated orthodontic appliances) were incubated in saline solution (0.05%), in shake, at 36ºC, for 60 days. The ion release was detected by atomic absorption spectrophotometer. The weight of brackets was also measured before and after the test. RESULTS: The results indicated that group A released more ions iron, nickel and chromium than group B. Moreover, the brackets in group A also presented weight loss, which is considered an indicator of corrosion. CONCLUSION: It was concluded that, under the present study conditions, the brackets from group A presented a higher biodegradation than group’s B brackets, what could be associated to composition and manufacturing process of these brackets.

O aço inoxidável austenítico é utilizado para confecção de dispositivos ortodônticos e contém cerca de 8-10% de níquel em sua composição, metal este responsável por reações alérgicas de hipersensibilidade. Acredita-se que a liberação de níquel dos dispositivos metálicos pode provocar dermatites de contato em pacientes suscetíveis. Este estudo laboratorial avaliou a influência de três variáveis na liberação de níquel: 1) o tipo de liga do braquete; 2) o tipo de solução de imersão e 3) o esforço mecânico nas canaletas dos braquetes de aço inoxidável austenítico. Foram avaliados seis grupos experimentais e dois grupos controles. As amostras foram imersas em tubos de ensaio contendo saliva artificial ou solução salina, sendo mantidas sob agitação e temperatura constante (37ºC). A quantidade de níquel presente nas soluções foi avaliada com espectrofotômetro de absorção atômica (Varian - Spectra A55) em dois momentos: após uma semana e após duas semanas. Os resultados revelaram que os braquetes de aço inoxidável com baixo teor de níquel apresentaram menor liberação deste elemento. Foi possível constatar que o tipo de solução alterou o padrão de liberação de níquel pelos dispositivos avaliados. O esforço mecânico aplicado sobre os braquetes de aço inoxidável austenítico não alterou a quantidade de níquel liberada.

Austenitic stainless steel is frequently used to fabricate orthodontic appliances, which contains 8-10% of nickel. Such metal is responsible for hypersensitivity allergic reactions. Thus, nickel release of orthodontic appliances may be responsible for contact dermatitis in sensitive patients. This study assessed the influence of three variables in nickel release of metal brackets: 1) type of metal alloy; 2) type of solution used for immersion; and 3) mechanical stress. Six experimental and two control groups were assessed. The specimens were immersed in saline solution or artificial saliva, maintained in constant agitation in controlled temperature environment (37ºC). Nickel present in solutions was measured with atomic spectroscopy (Varian-Spectra A55) in two moments: after one and after two weeks. The results showed that brackets made of low nickel contend alloy released less nickel than standard ones. It was possible to notice that the type of solution alters the pattern of nickel release. Mechanical stress applied in the slots of standard brackets did not influence nickel release.