Publicações

This set of articles describes the behaviour of formulated polyvinylchorides in various conditions of photoageing, including exposition in artificial and in natural conditions. In this article, the modification of the infrared and UVvisible spectra of PVC films irradiated with a xenon light are reported

One major problem encountered with polymeric materials is their sensitivity to outdoors weathering. Exposure to outdoors conditions leads to a degradation of the use properties of the material. This set of articles describes a comparison of the behavior of several stabilised polyvinylchlorides exposed to various conditions of ageing including light and temperature. The first article focusses on the effect of thermal ageing on the infrared and UV-visible characteristics of the selected samples.

This communication presents preliminary results of a research project on the effects of different environmental agents on the physical, chemical, aesthetical and mechanical properties of glass fibre reinforced polymer pultruded (GFRP) profiles made of either polyester or vinylester resin. In order to study the potential degradation of the two types of profiles in typical environments of civil engineering applications, test specimens are being subjected to the following exposure conditions: (i) immersion in demineralised water, at 23 ºC, 40 ºC and 60 ºC; (ii) immersion in salt-water, at the same temperatures; (iii) continuous condensation at 40 ºC; (iv) salt fog chamber; (v) thermal cycles, from -5ºC to 40ºC; (vi) accelerated weathering fluorescent ultraviolet light apparatus. Additionally, test specimens were placed in the roof of LNEC thereby being subjected to a natural degradation in a controlled environment. At predefined time intervals, batches of test specimens placed in the above mentioned exposure environments are being removed for physic-chemical and mechanical characterization, in order to assess their behaviour. / Nesta comunicação são apresentados os resultados preliminares de um projecto de investigação em que estão a ser avaliados os efeitos da degradação ambiental nas características físico-químicas de perfis pultrudidos de plástico reforçado com fibra de vidro com dois tipos de matriz – uma de poliéster e outra de viniléster. Com o objectivo de estudar os eventuais efeitos de degradação nos dois tipos de perfis, quando expostos a condições típicas das aplicações em engenharia civil, foram efectuadas as seguintes exposições em provetes retirados dos perfis: (i) imersão em água desmineralizada, a 23 ºC, 40 ºC e 60 ºC; (ii) imersão numa solução salina, às mesmas temperaturas; (iii) condensação em contínuo a 40 ºC; (iv) câmara de nevoeiro salino; (v) ciclos térmicos, entre -5 ºC e 40 ºC; (vi) envelhecimento artificial acelerado com lâmpadas fluorescentes de radiação ultravioleta. Para além disso, foram expostos provetes no telhado do edifício principal do LNEC, onde ficaram sujeitos a envelhecimento natural. Em intervalos predefinidos, foram efectuados ensaios de caracterização físico-química e mecânica dos materiais, para monitorizar o seu desempenho ao longo do tempo.

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The main purpose of this paper is to present the results of a study intended to assess the durability of stabilized PVC-U for outdoor applications, in form of calendered films and extruded plates. The samples were subject to different ageing conditions and their degradation state were evaluated, using techniques of molecular analysis, namely Fourier transformed infrared spectroscopy (FTIR), as well techniques for evaluation of macroscopic properties, as colorimetry and tensiles tests. The development of formulations, the ageing and the subsequent characterisation were done in LNEC. Therefore, after a brief introduction, this paper presents the experimental part of the study, as regards the composition of samples and the experimental methods of deterioration and characterisation. Subsequently, the results of the study, their interpretation and the final conclusions are also presented.

The main purpose of this paper is to present the results of a study intended to assess the durability of stabilized PVC-U for outdoor applications, in form of calendered films and extruded plates. The samples were subject to different ageing conditions and their degradation state were evaluated, using techniques of molecular analysis, namely Fourier transformed infrared spectroscopy (FTIR), as well techniques for evaluation of macroscopic properties, as colorimetry and tensiles tests. The development of formulations, the ageing and the subsequent characterisation were done in LNEC. Therefore, after a brief introduction, this paper presents the experimental part of the study, as regards the composition of samples and the experimental methods of deterioration and characterisation. Subsequently, the results of the study, their interpretation and the final conclusions are also presented.

The outdoor degradation of poly(vinyl chloride) (PVC) products is complex and not completely understood for most of the technical formulations. Furthermore, it is known that the behaviour of such materials is dependent of the photo-oxidation conditions, namely source of radiation, temperature, presence of water and humidity. In the present work, we have used X-ray photoelectron spectroscopy (XPS) to evaluate the influence of different photo-oxidation conditions on the surface degradation of stabilized PVC, low thickness calendered samples (~ 150 ?m). The main objective is the study of the influence of the weathering conditions on the degradation level of stabilized PVC products for outdoor applications trying to go deeper in the understanding of the mechanism of both the degradation and the stabilization of the surface under different environmental conditions, different polymer formulations and different processing methods (extrusion or calendering). Comparisons are made with previous results obtained using colourimetry and infrared spectroscopy. The role of PVC formulation and of radiation source and water were studied using artificial weathering. Results were compared with degradation induced by natural weathering in Lisbon.

The main purpose of this paper is to present the results obtained, during the years 2001 and 2002, from a study developed in LNEC. The object of this study was to assess the synergetic effect of three of the most significant deteriorating climatic agents (radiation, temperature and water) on the evolution of the properties of hard PVC stabilised with titanium dioxide, for outdoor applications. For the purpose, several samples were subject to natural and artificial weathering. Moreover, their physical and mechanical properties were characterised by techniques of analysis and assessment of the surface aspect (colour and brightness), of assessment of the molecular properties by infrared microscopy (MICROFTIR), as well as of determination of the tensile mechanical properties and assessment of the Charpy impact resistance. The paper was both orally presented and by poster at the panel meeting “Ageing, Irradiation, Stabilisation” of the Congress MoDeSt 2002. Therefore, this publication includes the text of the paper, the poster, as well as the slides from the oral communication. The development of the formulations, the ageing and the subsequent characterisation by colorimetry, brightness, Charpy impact and tension, were done in LNEC. The characterisation by infrared microscopy was performed in the Laboratoire de Photochimie Moleculaire et Macromoleculaire of the University Blaise-Pascal, Clermont-Ferrand, France.

The main purpose of this paper is to present the results obtained, during the year 2003, from a study developed in LNEC. The object of this study was to assess the synergetic effect of two deteriorating climatic agents (radiation and water) on the evolution of the properties of extruded plates made of hard PVC stabilised with titanium dioxide, for outdoor applications. For the purpose, several samples were subject to natural and artificial weathering, their deterioration condition having been characterised by means of techniques of analysis of colorimetry and infrared spectroscopy (FTIR). Initially, only the presentation of a poster titled “Artificial and Natural Weathering of Polyvinyl chloride for Outdoor Applications: the Influence of the Radiation and Water on the Evolution of the PVC Properties” was scheduled. Nevertheless, upon request from the secretariat of the Congress, the author also presented an oral paper on the same subject, but including experimental results obtained during the year 2004, which were not mentioned in the poster. Similarly, these results, which were obtained by means of surface analysis techniques by Scanning Electron Microscopy (SEM) and by X photoelectron spectroscopy (XPS), were not included in the paper submitted to the Congress. Therefore, this publication includes the text of the paper referring to the poster, which was initially predicted, as well as the slides of the oral communication presented. It also contains a few results obtained in 2004. The development of the formulations, as well as the ageing and the subsequent characterisation by colorimetry, by infrared spectroscopy and by scanning electron microscopy were performed in LNEC. The characterisation by X photoelectron spectroscopy was conducted at the Molecular Chemistry-Physics Centre of the Instituto Superior Técnico (Higher Technical Institute).

The main purpose of this paper is to present the results of a study intended to assess the deterioration condition of extruded hard PVC plates, for outdoor applications. The plates were subject to different ageing conditions, using techniques of surface analysis, namely scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The development of formulations, the ageing and the subsequent characterisation by scanning electron microscopy were done in LNEC. The characterisation by X-ray photoelectron spectroscopy was done at the Centre for Molecular Chemistry-Physics of Instituto Superior Técnico (Higher Technical Institute of Lisbon). Therefore, after a brief introduction, this paper presents the experimental part of the study, as regards the composition of samples and the experimental methods of deterioration and characterisation. Subsequently, the results of the study, their interpretation and the final conclusions are also presented.

Procurou-se com a presente comunicação, apresentar uma metodologia de validação de um programa informático, desenvolvido no NMPC do LNEC especificamente para a calibração de um calorimetro diferencial de varrimento (DSC) e para calcular a incerteza associada à determinação da entalpia de fusão. Assim, após uma breve introdução, a presente comunicação expõe a formulação essencial que serviu de suporte ao desenvolvimento do programa informático referido, descreve os elementos que constituem o procedimento de validação do mesmo, apresenta o processo de estimativa da incerteza de medição e os resultados da análise efectuada.

No presente relatório apresentam-se os dados meteorológicos do ano de 2007, recolhidos na estação meteorológica existente no Núcleo de Materiais Orgânicos do Departamento de Materiais do LNEC, em Lisboa.

Os resultados experimentais, obtidos através da medição de propriedades dos materiais e produtos, requerem tratamento específico e adequado, de forma a garantir a sua qualidade. É por isso muitas vezes necessário recorrer a métodos estatísticos para fazer a análise do tipo de distribuição dos resultados, proceder à deteção de valores suspeitos num conjunto de observações e à eventual rejeição de resultados anómalos. Este tipo de tratamento estatístico é principalmente adequado a ensaios de intercomparação, quer do foro metrológico (comparação de valores de padrões ou materiais de referência, mediante medição efetuada por operadores de diferentes laboratórios metrológicos, com incerteza variável), quer do âmbito dos laboratórios de ensaio. Os ensaios de Comparação Interlaboratorial realizados por laboratórios de ensaio, constituem uma ferramenta de garantia da Qualidade e são utilizados para a validação de métodos de ensaio (incerteza e robustez) e como um meio para a determinação das características de desempenho dos laboratórios, nomeadamente da reprodutibilidade e da repetibilidade. Nesta publicação faz-se uma descrição dos vários parâmetros que devem ser determinados em ensaios interlaboratoriais do tipo “Intercomparações com valor de consenso” e respetivos métodos de cálculo. A estatística aqui apresentada pode, numa boa parte dos casos, ser também aplicada à análise de resultados de medições experimentais correntes.

The main purpose of this Paper is to present a state of the art about weathering and polymer degradation. This review was presented during a training course promoted by the 5th European Weathering Symposium EWS (XXVIIth Colloquium of Danubian Countries on Natural and Artificial Ageing of Polymers), which was held in Lisbon on September 21 - 23, 2011, organised on behalf of CEEES (Confederation of European Environmental Engineering Societies) by the German Management Society for Environmental Engineering GUS (Gesellschaft für Umweltsimulation e.V.) and supported by SOPSAR (Sociedade Portuguesa de Simulação Ambiental e de Avaliação de Riscos), APIP (Associação Portuguesa da Indústria de Plásticos) and LNEC (Laboratório Nacional de Engenharia Civil). The main topics of this review are the weathering of polymers and composites, the determination, simulation and effects of relevant climatic quantities, innovative polymer additives, new test procedures and devices, instrumental methods of analysis to evaluate polymer degradation, recent developments in polymeric materials and composites designed for outdoor applications and methods for service-life prediction.

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