The partial least-squares (PLS) calibration method as a chemometric tool was used to develop a calibration model using Fourier transform infrared spectroscopy (FTIR) spectra data of biodiesel samples from different sources, such as cotton, castor, and palm, which were mixed with raw soybean oil to simulate an adulteration system. The PLS calibration method was applied with and without variable selection to quantify the amount of raw soybean oil present in these samples. Classic methods of variable selection, such as forward and stepwise, were applied to all origins together and each one separately. Variable selection improves not only the stability of the model to the colinearity in multivariate spectra but also the interpretability of the relationship between the model and the sample composition, which means that it becomes easier to determine and quantify the amount of raw soybean oil mixed in each biodiesel source.
Fodder radish;Raphanus sativus L. var. oleiferus Stokes;oil has been regarded as an interesting option to produce biodiesel, because the oil cannot be used for human consumption, the seeds have high oil content, and the cost of production is low. Furthermore, the plant has been used for green fertilization during the interval between harvests of other crops, due to its rapid development as well as its great ability to recycle nutrients. The content of free fatty acids in the crude oil is less than 0.5%, which makes it appropriate for basic catalyzed synthesis. However, basic catalyzed synthesis is very sensitive to the presence of water in the reaction environment. This study proposes the optimization of biodiesel synthesis using sodium ethoxide (sodium ethylate) as a catalyst, with the purpose of minimizing water formation during reaction, increase efficiency, and thus carry out transesterification in a single step. Ethanol was used instead of the methylic route, aiming at the production of an entirely renewable and environmentally preferable fuel. The experiments were proposed and carried out using a combination of fractional factorial design and Doehlert design, in order to allow an extensive study of the process variables with a minimum of experiments. Very intense levels of agitation and high temperatures proved to be inadequate to reach an effective reaction. At optimum conditions the ester content reached approximately 97.9%, which along with several other physical chemistry assays confirm the good quality of the product and that the synthesis of fodder radish crude oil can be performed in a single step efficiently.
Três origens diferentes de biodiesel (algodão, mamona e palma) foram adulteradas com óleo de soja cru, em concentrações variando de 1 a 40% (m/m). Estas amostras foram analisadas por espectrometria de infravermelho médio (MIR) e os seus espectros foram estudados em três diferentes faixas espectrais: espectro inteiro (4000-665 cm-1), e nas faixas de 1800-1700 cm-1 e 1800-1000 cm-1. Para determinar a origem do biodiesel utilizado no sistema adulterado, os dados espectrais foram analisados pela ferramenta análise de componentes principais (PCA) e a melhor segregação das origens foi obtida para o espectro inteiro (4000-665 cm-1). A variância explicada foi de 99%, para os três primeiros componentes. Para quantificar o óleo de soja cru foi aplicada a ferramenta mínimos quadrados parciais (PLS). Os melhores resultados foram obtidos para a região espectral de 1800-1000 cm-1 , com valores de RMSEP (erro médio quadrático de previsão) variando de 1,10 a 1,47% (m/m). Three different biodiesel sources (cotton, castor and palm) were adulterated with raw soybean oil at concentrations ranging from 1-40% (m/m). These samples were analyzed by infrared spectrometry (MIR) and their spectra were studied at three different spectral ranges: full spectrum (4000-665 cm-1), and the spectral ranges of 1800-1700 cm-1 and 1800-1000 cm-1. To determine the source of biodiesel used in the adulterated system, the data were analyzed by PCA (principal components analysis) spectral analysis tool and the best segregation of the sources was obtained at the range of 4000-665 cm-1. The explained variance was of 99% for the first three components. To quantify the raw soybean oil partial least squares (PLS) tool was applied. The best results were obtained for the spectral range of 1800-1000 cm-1 , with values of RMSEP (root mean square error of prediction) varying from 1.10 to 1.47% (m/m).
The aim of the present work was to verify the influence caused by the contamination or the addition of residual oil in the blends commercialized in Brazil [2% (v/v) of biodiesel in petrodiesel B2] in physicalchemistry parameters usually used to monitor the fuel quality, such as viscosity, flash point, distillation curve, specific gravity, and cetane index. To carry out the experiments, a set of samples simulating a system of fuel adulteration, mixing together biodiesel and residual oil, was prepared in concentrations varying from 0.5 to 25% (w/w). Then, these samples were submitted to the physical-chemistry assays cited before. The specific gravity presented itself as the most sensitive to adulteration. It detected the adulteration in concentration values of residual oil above 10% (w/w). Afterward, a calibration model was built using a multivariate calibration tool, partial least-squares (PLS), applied to attenuated total reflection/Fourier transformed infrared spectroscopy (ATR/FTIR) data to quantify the residual oil present in each sample. The PLS technique was shown to be very efficient in the determination of adulteration of B2 with residual oil from 0.5 to 25% (w/w).
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