The influence of temperature and pH on the ageing of piping made from polyamide 11 (PA-11) was studied using water from an oilfield (pH ¼ 5.5) and deionized water (pH ¼ 7.0) with monitoring by corrected inherent viscosity (CIV) measurements. The hydrolytic degradation was more extensive at high temperatures in oilfield water. When the system reaches equilibrium, the pH affects mainly the CIV plateau values. Thermogravimetry, energydispersive X-ray spectroscopy, differential scanning calorimetry, X-ray diffraction, and scanning electron microscopy measurements were also used to investigate aspects involved in the ageing PA-11. The hydrolytic degradation of PA-11 leads to formation of low molar mass compounds, such as oligomers dispersed in the polymeric matrix. This is a process that occurs preferentially in the amorphous domain of PA-11, which leads to an increase in the degree of crystallinity and the formation of a new c-phase.

This paper proposes the recycling of poly (methyl methacrylate) plates, formerly used in LCD monitors to produce polymer optical fibers without cladding for sensor systems and a discussion about the fabrication process of the fiber cladding is briefly presented. After disassembling LCD monitors the acrylic plate is cleaned and submitted to an extrusion process. Extrusion temperatures of 220°C, 230°C and 240°C were applied, and the produced polymer fibers were characterized by infrared and visible spectrometry, as well as evaluated for thermal analysis through differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). Furthermore, a refractive index sensor was developed with the recycled fibers. Results show that the recycled fiber refractive index sensor is linear (R = 0.99) and presents a sensitivity of more than 4 times higher when compared to a sensor using a commercial POF.

The influence of temperature (110 and 120 °C) on the ageing of piping made from polyamide 11 (PA‐11) containing 10–12% of plasticizer was studied using deionized water (pH ≈ 7.0). A clean analytical methodology has been employed for quality control of polymeric materials: energy‐dispersive X‐ray fluorescence spectrometry (ED‐XRF). It provides a fast and suitable technique to characterize chemical elements because of its multielemental capability, good sensitivity, high precision, short analytical time, and nondestructive nature. Herein, the content of additive in PA‐11 was monitored from ED‐XRF measurements where the abundance of the S line is directly related to the ageing time, agreeing with the thermogravimetric analysis. The XRF data were allied to chemometric treatment to classify PA‐11 samples according to the amount of additive and weight average molar mass change, predicting the ageing time, and viscosity values of PA‐11. Therefore, the XRF can be used as a clean analytical methodology to monitor the PA‐11 degradation, thus eliminating the use of toxic organic solvents (necessary to viscosity measurements) and reducing the working time. Also, the effect of hydrolysis on the structure over time and the material morphology were monitored through measurements of dynamic mechanical analysis and differential scanning calorimetry. Copyright © 2012 John Wiley & Sons, Ltd.

Resumo: O potencial da técnica de espectroscopia de infravermelho com transformada de Fourier e acessório de reflexão total atenuada (FTIR-ATR) foi avaliado para o monitoramento da degradação da poliamida 11 (PA-11) usada em dutos flexíveis. As amostras foram submetidas a envelhecimento em reatores com pressão controlada e atmosfera inerte. Os corpos de prova foram imersos em água deionizada (pH 7), nas temperaturas de 110, 120 e 140 °C por um período de até 50 dias. A técnica recomendada para monitoramento da degradação da PA-11 é a viscosimetria, através de medidas da viscosidade inerente corrigida (VIC) e a análise termogravimétrica (TGA). O comportamento observado para a VIC e TGA durante o envelhecimento possibilitou a construção de modelos que correlacionam com a técnica de FTIR-ATR. A partir dos resultados de FTIR-ATR, a variação na intensidade da banda atribuída à fase amorfa, 1161 cm -1 , possibilitou o monitoramento do envelhecimento quando associamos a técnica a modelos quimiométricos como o de regressão dos mínimos quadrados parciais, PLS. Portanto, a técnica FTIR-ATR pode ser uma nova alternativa no monitoramento da degradação hidrolítica da PA-11, eliminando assim o uso de solventes orgânicos tóxicos e reduzindo, consequentemente, o tempo de análise. Palavras-chave: Poliamida 11, PA-11, degradação, espectroscopia na região do infravermelho, FTIR-ATR. Monitoring the Degradation of Polyamide 11 (PA-11) via Fourier Transform Infrared Spectroscopy (FTIR)Abstract: The potential of the infrared spectroscopy with the attenuated total reflection technique (FTIR-ATR) was evaluated to monitor degradation of polyamide 11, PA-11, applied in flexible pipes. The samples were subjected to aging on reactors with controlled pressure and atmosphere. The samples were immersed in deionized water, pH 7, at temperatures of 110, 120 and 140 °C over a period of up to 50 days. The typical technique recommended for monitoring PA-11 degradation is viscometry from inherent viscosity corrected (VIC) and thermogravimetric (TGA) measurements. TGA and VIC results allowed the use of chemometric models that can be related to FTIR-ATR spectra, with assignment of a band to the amorphous phase (1161 cm -1 ) of PA-11. The chemometric model generated from PLS data was satisfactory in predicting the aging of PA-11. Therefore, FTIR-ATR can be used as a new analytical methodology to monitor PA-11 degradation, thus eliminating the use of toxic organic solvents and reducing the time required for the analysis. Keywords: Polyamide 11, PA-11, degradation, infrared spectroscopy, FTIR-ATR. IntroduçãoOs dutos flexíveis são estruturas fundamentais para o transporte do petróleo entre o poço situado ao fundo do oceano e as plataformas flutuantes de produção. Eles são capazes de acompanhar os grandes deslocamentos deste sistema. São vantajosos em relação aos dutos rígidos de aço, pois são fabricados em longos comprimentos e armazenados em carretéis, facilitando o transporte e a instalação [1] . Essas linhas flexíveis são estruturas multicamadas formad...

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