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Abstract: In this work, the use of 1H NMR spectroscopy and statistical approach to the evaluation of biodiesel–diesel blends quality is described. Forty-six mixtures of oil–diesel, biodiesel–diesel, and oil–biodiesel–diesel were analyzed by 1H NMR and such data were employed to design four predictive models. Thirty-six mixtures were used in the calibration set and the others in the validation. The PCR and PLS models were evaluated through statistical parameters. Briefly, PLS and PCR models were suitable for the prediction of biodiesel and oil concentration in mineral diesel. Specially, in higher concentration the predicted values were quite similar to the real ones. This fact was evidenced by the low relative errors of high concentrated samples; this means that the prediction of low concentrated samples will probably show high deviation. Therefore, 1H NMR-PLS and 1H NMR-PCR methods are fairly useful for the quality control of biodiesel–diesel blends, particularly they are suitable for prediction of concentrations greater than 2%. [Copyright &y& Elsevier]