Determination of mercury in rice by MSFIA and cold vapour atomic fluorescence spectrometry

In the present paper the use of a MSFIA system for determination of mercury in rice by cold vapour atomic fluorescence spectrometry (CV AFS) is proposed. The sample digestion is performed in a microwave oven using nitric acid and hydrogen peroxide. The experimental conditions for vapour generation were determined using a full two-level factorial design involving the following factors: nitric acid and tin chloride concentrations and sample flow rate. Employing the conditions optimised, the method allows the determination of mercury using the external calibration technique with aqueous standards. The reached limits of detection and quantification were 0.48 and 1.61 ng g−1 respectively, and the precision (as relative standard deviation) was 3.28% and 1.56% for rice samples with a mercury content of 3.63 and 5.81 ng g−1, respectively. The method accuracy was confirmed analysing a certified reference material of rice flour furnished by National Institute of Standard and Technology. The interference of nitrous acid and nitrous oxides are removed using potassium dichromate. The method was applied to mercury determination in twelve rice samples acquired in Palma de Mallorca (Spain) between the months of January and April of 2012. The mercury content found varied from 2.15 to 7.25 ng g−1. These results agree with those reported by others authors.

► It was proposed a method for determination of mercury by AFS using MSFIA.
► The method was applied in real samples.
► The method was completely validated.
► Factorial design was applied for optimization of the procedure.