Optimization of pretreatment procedure for MeHg determination in sediments and its applications

Methylmercury (MeHg) in sediment is difficult to be determined due to its low concentration and binding compounds like sulfide and organic matter. Moreover, wet sediment samples have been suggested to behave differently from certified reference materials in MeHg analysis. Optimal pretreatment procedure for MeHg determination in sediments has not been ascertained and whether the procedure could apply to sediment samples with complex matrix merits further research. This work firstly compared recovery results of five pretreatment procedures for MeHg determination using ERM-CC580. Using the optimal pretreatment procedure, recovery results were analyzed in different sediment samples after manipulation of moisture content, organic matter, and acid volatile sulfide. The procedure using CuSO4/HNO3 as leaching solutions and mechanical shaking as extraction method was proved to produce the most satisfactory recovery results (100.67 ± 6.75%, mean ± standard deviation). And when moisture content varied from 20 to 80%, average recovery results in sediment samples ranged from 100 to 125%. Furthermore, before and after the manipulation of organic matter or acid volatile sulfide, spiking recovery results varied little and were all within acceptable limit (85~105%). Therefore, the procedure of CuSO4/HNO3-mechanical is proposed as a universal pretreatment method for MeHg determination in sediment samples with various characteristics.