Removal of sulfamethoxazole from solution by raw and chemically treated walnut shells

Purpose: The sorption of sulfamethoxazole, a frequently detected pharmaceutical compound in the environment, onto walnut shells was evaluated. Methods: The sorption proprieties of the raw sorbent were chemically modified and two additional samples were obtained, respectively HCl and NaOH treated. Scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and thermogravimetric (TG/DTG) techniques were applied to investigate the effect of the chemical treatments on the shell surface morphology and chemistry. Sorption experiments to investigate the pH effect on the process were carried out between pH 2 and 8. Results: The chemical treatment did not substantially alter the structure of the sorbent (physical and textural characteristics) but modified the surface chemistry of the sorbent (acid–base properties, point of zero charge—pHpzc). The solution pH influences both the sorbent’s surface charge and sulfamethoxazole speciation. The best removal efficiencies were obtained for lower pH values where the neutral and cationic sulfamethoxazole forms are present in the solution. Langmuir and Freundlich isotherms were applied to the experimental adsorption data for sulfamethoxazole sorption at pH 2, 4, and 7 onto raw walnut shell. No statistical difference was found between the two models except for the pH 2 experimental data to which the Freundlich model fitted better. Conclusion: Sorption of sulfamethoxazole was found to be highly pH dependent in the entire pH range studied and for both raw and treated sorbent.

Preparação de catalisadores heterogéneos para a produção de biodiesel

A produção de biodiesel como combustível para motores diesel, aumentou fortemente nos últimos anos e espera-se que cresça mais e mais num futuro próximo. O aumento do consumo de biodiesel exige processos de produção optimizados que permitam grandes capacidades de produção, operações simplificadas, rendimentos altos, bem como a utilização de matérias-primas mais económicas. Por isso, o desenvolvimento de processos de produção de baixo custo exige a especificação de catalisadores heterogéneos eficientes na promoção da reacção de transesterificação, permitindo a imediata separação da glicerina pura, não necessitando de uma purificação dispendiosa deste subproduto. Os xerogéis de carbono surgem então como materiais promissores para aplicação como catalisadores heterogéneos para a produção de biodiesel, devido às suas excelentes propriedades ao nível da sua textura e superfície química. Neste trabalho o principal objectivo foi a preparação de um xerogel de carbono, com o intuito de posteriormente ser aplicado na produção de biodiesel por catálise heterogénea. Amostras de xerogel de carbono foram preparadas pelo método sol-gel e oxidadas em fase líquida sendo posteriormente caracterizados os seus grupos funcionais e a sua área específica. Os resultados obtidos mostram que é possivel obter um xerogel de carbono com área superficial alta, tendo sido atingido um valor máximo para a amostra número dois (803 m2/g). Os resultados atingidos ao nível da preparação do catalisador permitem concluir que as condições de operação influenciam a estrutura final do xerogel de carbono. Quanto à caracterização da química superficial do xerogel, foi possível verificar que a diferença do número de acidez entre as amostras oxidadas e não oxidadas do mesmo lote é alta, o que permite afirmar que a oxidação do material de carbono incrementa a concentração de grupos oxigénio à superfície do xerogel. O valor máximo para o número de acidez foi obtido com a amostra número três (Amostra oxidada - 916 μmol/g, Amostra não oxidada - 207 μmol/g). Apesar de terem sido realizados ensaios para a produção de biodiesel os resultados obtidos foram nulos. A escolha das condições de reacção para a catálise heterogénea com este tipo de material poderá não ter sido a mais indicada, assim como a quantidade e o tipo de grupos funcionais introduzidos no catalisador não terem acidez suficiente para permitir uma catálise efectiva.

Preparação de adsorventes mesoporosos para a adsorção de poluentes em águas

Mestrado Engenharia Química. Ramo Tecnologias de Protecção Ambiental

Sol-Gel Chemistry in Biosensing Devices of Electrical Transduction: Application to CEA Cancer Biomarker

Sol-gel chemistry allows the immobilization of organic molecules of biological origin on suibtable solid supports, permitting their integration into biosensing devices widening the possibility of local applications. The present work is an application of this principle, where the link between electrical receptor platform and the antibody acting as biorecognition element is made by sol-gel chemistry. The immunosensor design was targeted for carcinoembryonic antigen (CEA), an important biomarker for screening the colorectal cancer, by electrochemical techniques, namely electrochemical impedance spectroscopy (EIS) and square wave voltammetry (SVW). The device displayed linear behavior to CEA in EIS and in SWV assays ranging from 0.50 to 1.5ng/mL, and 0.25 to 1.5ng/mL, respectively. The corresponding detection limits were 0.42 and 0.043 ng/mL. Raman spectroscopy was used to characterize the surface modifications on the conductive platform (FTO glass). Overall, simple sol-gel chemistry was effective at the biosensing design and the presented approach can be a potential method for screening CEA in point-of-care, due to the simplicity of fabrication, short response time and low cost. - See more at: http://www.eurekaselect.com/127192/article#sthash.m1AWhINx.dpuf

Backside-surface imprinting as a new strategy to generate specific plastic antibody materials

A backside protein-surface imprinting process is presented herein as a novel way to generate specific synthetic antibody materials. The template is covalently bonded to a carboxylated-PVC supporting film previously cast on gold, let to interact with charged monomers and surrounded next by another thick polymer. This polymer is then covalently attached to a transducing element and the backside of this structure (supporting film plus template) is removed as a regular “tape”. The new sensing layer is exposed after the full template removal, showing a high density of re-binding positions, as evidenced by SEM. To ensure that the templates have been efficiently removed, this re-binding layer was cleaned further with a proteolytic enzyme and solution washout. The final material was named MAPS, as in the back-side reading of SPAM, because it acts as a back-side imprinting of this recent approach. It was able to generate, for the first time, a specific response to a complex biomolecule from a synthetic material. Non-imprinted materials (NIMs) were also produced as blank and were used as a control of the imprinting process. All chemical modifications were followed by electrochemical techniques. This was done on a supporting film and transducing element of both MAPS and NIM. Only the MAPS-based device responded to oxLDL and the sensing layer was insensitive to other serum proteins, such as myoglobin and haemoglobin. Linear behaviour between log(C, μg mL−1) versus charged tranfer resistance (RCT, Ω) was observed by electrochemical impedance spectroscopy (EIS). Calibrations made in Fetal Calf Serum (FCS) were linear from 2.5 to 12.5 μg mL−1 (RCT = 946.12 × log C + 1590.7) with an R-squared of 0.9966. Overall, these were promising results towards the design of materials acting close to the natural antibodies and applied to practical use of clinical interest.