Pelchem, a commercial subsidiary of Necsa (South African Nuclear Energy Corporation), produces a range of commercial fluorocarbon products while driving research and development initiatives to support the fluorine product portfolio. One such initiative is to develop improved analytical techniques to analyse product composition during development and to quality assure produce. Generally the C–F type products produced by Necsa are in a solution of anhydrous HF, and cannot be directly analyzed with traditional techniques without derivatisation. A technique such as vibrational spectroscopy, that can analyze these products directly without further preparation, will have a distinct advantage. However, spectra of mixtures of similar compounds are complex and not suitable for traditional quantitative regression analysis. Multivariate data analysis (MVA) can be used in such instances to exploit the complex nature of spectra to extract quantitative information on the composition of mixtures. A selection of fluorocarbon alcohols was made to act as representatives for fluorocarbon compounds. Experimental design theory was used to create a calibration range of mixtures of these compounds. Raman and infrared (NIR and ATR–IR) spectroscopy were used to generate spectral data of the mixtures and this data was analyzed with MVA techniques by the construction of regression and prediction models. Selected samples from the mixture range were chosen to test the predictive ability of the models. Analysis and regression models (PCR, PLS2 and PLS1) gave good model fits (R2 values larger than 0.9). Raman spectroscopy was the most efficient technique and gave a high prediction accuracy (at 10% accepted standard deviation), provided the minimum mass of a component exceeded 16% of the total sample. The infrared techniques also performed well in terms of fit and prediction. The NIR spectra were subjected to signal saturation as a result of using long path length sample cells. This was shown to be the main reason for the loss in efficiency of this technique compared to Raman and ATR–IR spectroscopy. It was shown that multivariate data analysis of spectroscopic data of the selected fluorocarbon compounds could be used to quantitatively analyse mixtures with the possibility of further optimization of the method. The study was a representative study indicating that the combination of MVA and spectroscopy can be used successfully in the quantitative analysis of other fluorocarbon compound mixtures. / Thesis (M.Sc. (Chemistry))--North-West University, Potchefstroom Campus, 2012.

Pelchem, a commercial subsidiary of Necsa (South African Nuclear Energy Corporation), produces a range of commercial fluorocarbon products while driving research and development initiatives to support the fluorine product portfolio. One such initiative is to develop improved analytical techniques to analyse product composition during development and to quality assure produce. Generally the C–F type products produced by Necsa are in a solution of anhydrous HF, and cannot be directly analyzed with traditional techniques without derivatisation. A technique such as vibrational spectroscopy, that can analyze these products directly without further preparation, will have a distinct advantage. However, spectra of mixtures of similar compounds are complex and not suitable for traditional quantitative regression analysis. Multivariate data analysis (MVA) can be used in such instances to exploit the complex nature of spectra to extract quantitative information on the composition of mixtures. A selection of fluorocarbon alcohols was made to act as representatives for fluorocarbon compounds. Experimental design theory was used to create a calibration range of mixtures of these compounds. Raman and infrared (NIR and ATR–IR) spectroscopy were used to generate spectral data of the mixtures and this data was analyzed with MVA techniques by the construction of regression and prediction models. Selected samples from the mixture range were chosen to test the predictive ability of the models. Analysis and regression models (PCR, PLS2 and PLS1) gave good model fits (R2 values larger than 0.9). Raman spectroscopy was the most efficient technique and gave a high prediction accuracy (at 10% accepted standard deviation), provided the minimum mass of a component exceeded 16% of the total sample. The infrared techniques also performed well in terms of fit and prediction. The NIR spectra were subjected to signal saturation as a result of using long path length sample cells. This was shown to be the main reason for the loss in efficiency of this technique compared to Raman and ATR–IR spectroscopy. It was shown that multivariate data analysis of spectroscopic data of the selected fluorocarbon compounds could be used to quantitatively analyse mixtures with the possibility of further optimization of the method. The study was a representative study indicating that the combination of MVA and spectroscopy can be used successfully in the quantitative analysis of other fluorocarbon compound mixtures. / Thesis (M.Sc. (Chemistry))--North-West University, Potchefstroom Campus, 2012.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / This study aims to investigate chemical, physical, mechanical and surface properties of Eucalyptus grandis and Eucalyptus cloeziana wood subjected to different treatments of freezing and heat. To achieve this, six trees for each specie were used to prepare sample for each mechanical test. The samples were subjected to six thermal treatments. Freezing treatment was performed in a horizontal freezer at -22 ± 2°C for 72 hours, while heat treatment was performed using an oven with force air circulation at 180 and 200 ± 1°C for 3.5 hours. Sampling to perform chemical, physical and surface tests were obtained from samples used in mechanical characterization of wood. Chemical changes were evaluated quantitatively through wet process and qualitatively through infrared spectroscopy (ATR-IR). Physical properties evaluated were: weight loss, specific gravity, equilibrium moisture content, dimensional stability and hygroscopicity of wood. Mechanical evaluation was performed through static bending, impact strength, compression parallel to fibers and Janka hardness. Color and wettability of wood were evaluated using colorimetry and contact angle techniques, respectively. The main findings showed that freezing slightly affected the chemical properties of wood, in which the main changes were found in heat treatments, mainly at 200°C. Freezing improve in weight and equilibrium moisture content of wood, while heat treatment caused weight loss and decrease of equilibrium moisture content of wood. Both heat treatments improved dimensional stability of wood, however when freezing and heat was performed in a combination, they did not showed the best results. Regarding the hygroscopicity of wood, results obtained in heat treatment at 200°C should be highlighted. On the other hand, freezing treatment increased absorption of water. In general, freezing reduced mechanical properties of wood. Heat treatments increased stiffness at static bending and strength at compression parallel to fibers of wood however was responsible for reduction in other mechanical properties. Color of wood was affected mainly for heat treatments, in which a darkening of surface was observed and quantified by decrease of parameter L*. Wettability of wood slightly decreased after heat treatments. Influence of freezing on wettability of wood was related to the natural characteristic of wood from species studied because they did not showed a defined tendency. Therefore, it is believed that treatments performed in this study changed significantly the technological properties of wood. / O presente estudo teve como objetivos investigar as propriedades químicas, físicas, mecânicas e superficiais da madeira de Eucalyptus grandis e Eucalyptus cloeziana submetida a diferentes tratamentos de congelamento e termorretificação. Para tanto, foram confeccionados, a partir de seis árvores de cada espécie, corpos de prova para cada ensaio mecânico. Os corpos de prova foram submetidos a seis tratamentos térmicos. O congelamento foi realizado em um freezer horizontal sob condições de temperatura e tempo de -22 ± 2°C durante 72 horas, enquanto que a termorretificação foi realizada em uma estufa laboratorial com circulação de ar forçada, à 180 e 200 ± 1°C durante 3,5 horas. A amostragem para realização dos ensaios químicos, físicos e superficiais foram provenientes dos corpos de prova utilizados na caracterização mecânica da madeira. As modificações químicas foram avaliadas quantitativamente em ensaios via úmida e qualitativamente por espectroscopia no infravermelho (ATR-IR). As propriedades físicas avaliadas foram a perda de massa e massa específica, teor de umidade de equilíbrio, estabilidade dimensional e higroscopicidade da madeira. Para avaliação das propriedades mecânicas foram realizados ensaios de flexão estática, flexão dinâmica, compressão paralela e dureza Janka. Também foram avaliadas a colorimetria e molhabilidade da madeira, por meio das técnicas de colorimetria e ângulo de contato. Os principais resultados encontrados mostraram que o congelamento pouco afetou as propriedades químicas da madeira, sendo as principais alterações oriundas do processo de termorretificação, principalmente a 200°C. O congelamento causou acréscimos na massa e no teor de umidade de equilíbrio da madeira, enquanto que a termorretificação ocasionou a perda de massa e redução do teor de umidade de equilíbrio. Os dois tratamentos térmicos causaram melhoria na estabilidade dimensional, entretanto, quando combinados, não apresentaram os melhores resultados. Para a higroscopicidade destacam-se os resultados obtidos na termorretificação a 200°C, por outro lado, o congelamento aumentou a absorção de água. De maneira geral, o congelamento causou redução nas propriedades mecânicas da madeira. A termorretificação causou aumento na rigidez a flexão estática e resistência a compressão paralela e redução nas demais propriedades mecânicas. A coloração da madeira foi afetada principalmente pela termorretificação, em que ocorreu um escurecimento superficial, quantificado pelo decréscimo do parâmetro de claridade L*. A molhabilidade da madeira diminuiu sensivelmente após a realização dos tratamentos de termorretificação. A influência do congelamento sobre a molhabilidade foi atribuída a características naturais da madeira das espécies estudadas, sem apresentar tendência definida. Dessa forma, verificou-se que os tratamentos realizados alteraram significativamente as propriedades tecnológicas da madeira.