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Este trabalho apresenta o desenvolvimento e a validação de dois modelos PLS para quantificação de biodiesel metílico e biodiesel etílico provenientes de óleos de fritura em misturas com diesel empregando dados de espectroscopia no infravermelho médio. A exatidão dos modelos PLS mostraram excelente desempenho com baixos valores de RMSEC, RMSECV e RMSEP. Além disso, a exatidão foi comprovada pela avaliação da região de elipse de confiança. O método foi validado de acordo com as diretrizes internacionais e nacionais pela estimativa de figuras de mérito, tais como exatidão, precisão, linearidade, seletividade, sensibilidade analítica, limites de detecção e quantificação e erro sistemático. Uma excelente correlação foi observada entre os valores reais e previstos do conjunto de previsão (R = 0,9999) e os modelos não apresentaram erros sistemáticos conforme a norma ASTM E1655. Os modelos propostos utilizam uma única faixa espectral permitindo a determinação de biodiesel em mistura com diesel na faixa de concentração entre 1,00 e 30,00% (v/v), em ambos os modelos. Assim, as metodologias propostas foram validadas sem a necessidade de escolher faixas espectrais se comparado com as normas pertinentes que regulamentam a determinação do teor de biodiesel em mistura com diesel. DOI: 10.5935/1984-6835.20140098This study presents the development and validation of two PLS models for quantification of methyl and ethyl biodiesels from waste frying oils in diesel blends by mid-infrared spectroscopy. The accuracy of the PLS models showed excellent performance by presenting low values of RMSEC, RMSECV and RMSEP. The PLS models provided RMSEC of 0.07% (v/v) and 0.04% (v/v) for the models containing methyl and ethyl biodiesels, respectively; and RMSEP of 0.09% (v/v) and 0.05% (v/v). Addition to the parameters of error it was evaluated the accuracy by elliptical joint confidence region. The method was validated according to international and national guidelines by the estimation of figures of merit, such as accuracy, precision, linearity, selectivity, analytical sensitivity, limits of detection and quantification and systematic error. An excellent correlation was observed in prediction set (R = 0.9999), and no systematic errors were present according to the ASTM E1655 standard. The proposed models for the entire spectral region allowed the determination of both methyl and ethyl biodiesels from waste frying oil in diesel using concentrations between 1.00 and 30.00% (v/v). The proposed methodologies were validated and no need for selecting intervals if compared with relevant standards that regulate the determination of biodiesel blend levels in diesel. DOI: 10.5935/1984-6835.2014009

Development and Validation of PLS Models for Quantification of Biodiesels Content from Waste Frying Oil in Diesel by HATR-MIR