Abstract

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This paper describes the validation of the method for determination of total mercury in petroleum coke samples by cold vapor atomic fluorescence spectrometry after sample treatment for green coke by procedure assisted by microwave. In this context, some validation parameters are evaluated as metrological tools to improve the methodology. The method has been validated in accordance with international protocols and suitable parameters were evaluated as accuracy, precision, linearity, detection e quantification limits, sensitivity, working range and uncertainty of measurement. Limits of detection and quantification have been used to compare different regression models: the Ordinary Least Squares Method and Weighted Least Squares Method. In addition, the evaluation of uncertainty of measurement and error sources allowed the measuring the errors sources contribution and its mapping. The method was applied to ten green coke samples and the results showed that the total mercury concentration in green petroleum coke was between 0.110 and 0.201 mg kg^-1 ,which is very low to be detected for the majority of the analytical techniques. The evaluation of the validation parameters has proved that the proposed method has satisfactory performance.