Anodic adsorptive stripping voltammetric determination of atrazine in spiked soil samples with a gold microelectrode

Microwave-assisted solvent extraction was combined with anodic adsorptive stripping voltammetry at a gold microelectrode to extract and quantify the herbicide atrazine in spiked soil samples. A systematic study of the experimental parameters affecting the stripping response was carried out by square-wave voltammetry. The voltammetric procedure is based on controlled adsorptive accumulation of atrazine at the potential of 0.35V (versus Ag/AgCl) in the presence of Britton–Robinson buffer pH (2.0). The limit of detection obtained for a 30 sec collection time was 4.3x10-7 mol L-1. Recovery experiments, at the 1µgg-1 level of spiking, gave good results for the global procedure, and the values found were comparable to those obtained by HPLC.

Rapid determination of tartaric acid in wines

A flow-spectrophotometric method is proposed for the routine determination of tartaric acid in wines. The reaction between tartaric acid and vanadate in acetic media is carried out in flowing conditions and the subsequent colored complex is monitored at 475 nm. The stability of the complex and the corresponding formation constant are presented. The effect of wavelength and pH was evaluated by batch experiments. The selected conditions were transposed to a flowinjection analytical system. Optimization of several flow parameters such as reactor lengths, flow-rate and injection volume was carried out. Using optimized conditions, a linear behavior was observed up to 1000 µg mL-1 tartaric acid, with a molar extinction coefficient of 450 L mg-1 cm-1 and ± 1 % repeatability. Sample throughput was 25 samples per hour. The flow-spectrophotometric method was satisfactorily applied to the quantification of tartaric acid (TA) in wines from different sources. Its accuracy was confirmed by statistical comparison to the conventional Rebelein procedure and to a certified analytical method carried out in a routine laboratory.

Development of a SPME-GC-ECD methodology for selected pesticides in must and wine samples

A method for the determination of some pesticide residues in must and wine samples was developed using solid-phase microextraction (SPME) and gas chromatography – electron capture detection (GC/ECD). The procedure only needs dilution as sample pre-treatment and is therefore simple, fast and solvent-free. Eight fungicides (vinclozolin, procymidone, iprodione, penconazole, fenarimol, folpet, nuarimol and hexaconazole), one insecticide (chlorpyriphos) and two acaricides (bromopropylate and tetradifon) can be quantified. Good linearity was observed for all the compounds in the range 5–100 µg/L. The reproducibility of the measurements was found acceptable (with RSD’s below 20%). Detection limits of 11 µg/L, on average, are sufficiently below the proposed maximum residue limits (MRL’s) for these compounds in wine. The analytical method was applied to the determination of these compounds in Portuguese must and wine samples from the Demarcated Region of Alentejo, where any residues could be detected.

Optimization of QuEChERS procedure coupled to GC-ECD for organochlorine pesticide determination in carrot samples

An optimised version of the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for simultaneous determination of 14 organochlorine pesticides in carrots was developed using gas chromatography coupled with electron-capture detector (GC-ECD) and confirmation by gas chromatography tandem mass spectrometry (GC-MS/MS). A citrate-buffered version of QuEChERS was applied for the extraction of the organochlorine pesticides, and for the extract clean-up, primary secondary amine, octadecyl-bonded silica (C18), magnesium sulphate (MgSO4) and graphitized carbon black were used as sorbents. The GC-ECD determination of the target compounds was achieved in less than 20 min. The limits of detection were below the EUmaximum residue limits (MRLs) for carrots, 10–50 μg kg−1, while the limit of quantification did exceed 10 μg kg−1 for hexachlorobenzene (HCB). The introduction of a sonication step was shown to improve the recoveries. The overall average recoveries in carrots, at the four tested levels (60, 80, 100 and 140 μg kg−1), ranged from 66 to 111% with relative standard deviations in the range of 2– 15 % (n03) for all analytes, with the exception of HCB. The method has been applied to the analysis of 21 carrot samples from different Portuguese regions, and β-HCH was the pesticide most frequently found, with concentrations oscillating between less than the limit of quantification to 14.6 μg kg−1. Only one sample had a pesticide residue (β-HCH) above the MRL, 14.6 μg kg−1. This methodology combines the advantages of both QuEChERS and GC-ECD, producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.

Response surface methodology applied to SPE for the determination of ibuprofen in various types of water samples

Over the last few years, there has been a growing concern about the presence of pharmaceuticals in the environment. The main objective of this study was to develop and validate an SPE method using surface response methodology for the determination of ibuprofen in different types of water samples. The influence of sample pH and sample volume on the ibuprofen recovery was studied. The effect of each studied independent variable is pronounced on the dependent variable (ibuprofen recovery). Good selectivity, extraction efficiency, and precision were achieved using 600 mL of sample volume with the pH adjusted to 2.2. LC with fluorescence detection was employed. The optimized method was applied to 20 water samples from the North and South of Portugal.

An integrated reusable remote laboratory to complement electronics teaching

The great majority of the courses on science and technology areas where lab work is a fundamental part of the apprenticeship was not until recently available to be taught at distance. This reality is changing with the dissemination of remote laboratories. Supported by resources based on new information and communication technologies, it is now possible to remotely control a wide variety of real laboratories. However, most of them are designed specifically to this purpose, are inflexible and only on its functionality they resemble the real ones. In this paper, an alternative remote lab infrastructure devoted to the study of electronics is presented. Its main characteristics are, from a teacher's perspective, reusability and simplicity of use, and from a students' point of view, an exact replication of the real lab, enabling them to complement or finish at home the work started at class. The remote laboratory is integrated in the Learning Management System in use at the school, and therefore, may be combined with other web experiments and e-learning strategies, while safeguarding security access issues.

Extended immersive learning environment: a hybrid remote/virtual laboratory

This paper presents a collaborative virtual learning environment, which includes technologies such as 3D virtual representations, learning and content management systems, remote experiments, and collaborative learning spaces, among others. It intends to facilitate the construction, management and sharing of knowledge among teachers and students, in a global perspective. The environment proposes the use of 3D social representations for accessing learning materials in a dynamic and interactive form, which is regarded to be closer to the physical reality experienced by teachers and students in a learning context. A first implementation of the proposed extended immersive learning environment, in the area of solid mechanics, is also described, including the access to theoretical contents and a remote experiment to determine the elastic modulus of a given object.These instructions give you basic guidelines for preparing camera-ready papers for conference proceedings. Use this document as a template if you are using Microsoft Word 6.0 or later. Otherwise, use this document as an instruction set. The electronic file of your paper will be formatted further. Define all symbols used in the abstract. Do not cite references in the abstract.

Determinação do teor de compostos aromáticos policíclicos de óleos minerais isolantes para transformadores

Mestrado em Engenharia Química - Ramo Optimização Energética na Indústria Química

Diagnóstico de funcionamento e otimização das ETARs do concelho da Póvoa de Varzim

O tratamento das águas residuais é uma matéria de extrema importância para o município da Póvoa de Varzim, não só por uma questão de saúde pública e conservação do meio ambiente como também pela vertente turística deste concelho, que tem na sua orla costeira seis praias às quais foram atribuídas bandeiras azuis pela sua qualidade. O concelho da Póvoa de Varzim engloba doze freguesias e possui quinze estações de tratamento de águas residuais (ETARs), sendo catorze delas compactas. O seu controlo é assegurado pela divisão de saneamento básico da câmara municipal da Póvoa de Varzim. O objetivo deste trabalho foi o diagnóstico de funcionamento das ETARs do município tendo em vista a identificação dos problemas existentes e a sua resolução/otimização. De forma a poder identificar o princípio de funcionamento e a presença de anomalias nas estações de tratamento, foram realizadas várias visitas a cada uma delas ao longo do período de estágio. A recolha de amostras para análises dos diferentes parâmetros foi feita por um funcionário e estas foram enviadas para o laboratório com parceria com a Câmara Municipal. Após uma extensa recolha de informação no local e de um estudo exaustivo de toda a documentação associada a cada ETAR concluiu-se que apenas quatro delas apresentavam problemas revelantes. As ETARs do parque industrial de Laúndos e do centro histórico de Rates apresentam caudais de admissão bastante elevados devido à descarga pontual de camiões cisterna o que faz com que o tratamento não seja eficaz. Como solução sugeriu-se a construção de um tanque de equalização em ambas as ETARs, com agitador e regulador de caudal, de forma a garantir, respetivamente, a mistura e uniformização das águas residuais domésticas e industriais e que apenas será bombeado o caudal adequado para tratamento. As ETARs da Incondave e das Fontaínhas apresentam sobretudo anomalias a nível do equipamento, o que leva a um mau desempenho da instalação. Aconselhou-se o conserto dos equipamentos danificados e uma inspeção mais frequente das instalações para que mal ocorra uma avaria, esta seja reparada o mais depressa possível. O estágio na câmara municipal da Póvoa de Varzim (CMPV) teve a duração de 10 meses, entre Outubro e Julho de 2012 e foi realizado no âmbito da disciplina de dissertação/ estágio do mestrado de tecnologias de proteção ambiental no Instituto Superior de Engenharia do Porto. Este estágio foi uma mais-valia para mim na medida em que pude consolidar os conhecimentos adquiridos ao longo de todo o meu percurso académico e conhecer a realidade do mercado de trabalho.