Determination of mercury in estuarine sediments by flow injection-cold vapour atomic absorption spectrometry after microwave extraction

Abstract

A flow injection-cold vapour atomic absorption spectrometric (CVAAS) method was developed for the determination of mercury at trace level in estuarine sediments using sodium tetrahydroborate (III) as reductant. The mercury was solubilized with nitric acid in closed vessels and microwave oven heating. Instrumental and operational conditions (volume and concentration of reagents, reaction time, etc.) were optimized. The effect of several ions on the analytical signal was also studied; no interferences were recorded excepting for copper and nickel which caused a serious depressing effect. The detection limit obtained was 0.01 μg g -1 . The validation of the method was performed analyzing a certified reference sediment, BCR CRM 277 Estuarine Sediment. Good recovery (c.a. 98%) and precision (< 3%, RSD) were achieved. The proposed method was successfully applied to the determination of mercury in sediment samples from Ares-Betanzos Estuary (Galicia, NW Spain).