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A statistical procedure to validate an analytical methodology by standard addition methodology is described. The data set obtained in 3 calibration experiments with standard solutions, standard additions, and portions of sample is used. The accuracy of the analytical results is checked by comparison of analyte contents in the different calibrations and from the recovery. Mathematical expressions to estimate the statistical parameters are proposed. The statistical protocol has been applied to fluorimetric determination of molybdenum with alizarin S in vegetable tissues.

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