Method development and sample processing of water, soil, and tissue for the analysis of total and organic mercury by cold vapor atomic fluorescence spectrometry

Atomic Fluorescence-based methods have been developed for measuring ultratrace levels of mercury (Hg) in environmental (water, soil) and biological (fish tissue) samples. In addition, methods for preparation of water, soil, and tissue samples have been developed. For the analysis of total Hg in soil, sediment and fish the samples are digested with concentrated nitric acid in sealed glass ampules, and subsequently autoclaved. Water samples are digested using standard brominating procedures. A Merlin Plus, PS Analytical atomic fluorescence spectrometer (AFS) system equipped with an autosampler, vapor generator, fluorescence detector and a PC based integrator package is used in the determination of total Hg. The determination of Hg mercury species in water, without pre-derivatization, involves adsorbent pre-concentration of the organomercurials onto sulfydryl-cotton fibers. The organic Hg compounds are eluted with a small volume of acidic KBr and CuSO sub(4) and extracted into dichloromethane. Sediment, soil and tissue samples are homogenized and the organomercurials first released from the sample by the combined action of acidic KBr and CuSO sub(4) and extracted into dichloromethane. The initial extracts are subjected to thiosulfate clean-up and the organomercury species are isolated as their chloride derivatives by cupric chloride addition and subsequent extraction into a small volume of dichloromethane. Analysis of organic Hg compounds is accomplished by capillary column chromatography coupled with atomic fluorescence detection.