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U.S. GEOLOGICAL SURVEY Open-File Report 01-445
Version 1.0

Determination of Methyl Mercury by Aqueous Phase Ethylation, Followed by Gas Chromatographic Separation with Cold Vapor Atomic Fluorescence Detection

By John F. De Wild, Mark L. Olson, and Shane D. Olund

Abstract

A recent national sampling of streams in the United States revealed low methyl mercury concentrations in surface waters. The resulting median and mean concentrations, calculated from 104 samples, were 0.06 nanograms per liter (ng/L) and 0.15 ng/L, respectively. This level of methyl mercury in surface water in the United States has created a need for analytical techniques capable of detecting sub-nanogram per liter concentrations. In an attempt to create a U.S. Geological Survey approved method, the Wisconsin District Mercury Laboratory has adapted a distillation/ethylation/ gas-phase separation method with cold vapor atomic fluorescence spectroscopy detection for the determination of methyl mercury in filtered and unfiltered waters. This method is described in this report. Based on multiple analyses of surface-water and ground-water samples, a method detection limit of 0.04 ng/L was established. Precision and accuracy were evaluated for the method using both spiked and unspiked ground-water and surface- water samples. The percent relative standard deviations ranged from 10.2 to 15.6 for all analyses at all concentrations. Average recoveries obtained for the spiked matrices ranged from 88.8 to 117 percent. The precision and accuracy ranges are within the acceptable method-performance limits. Considering the demonstrated detection limit, precision, and accuracy, the method is an effective means to quantify methyl mercury in waters at or below environmentally relevant concentrations.

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Send questions or comments about this report to the author, John DeWild, (608) 821-3846.

For more information, visit the USGS Mercury Research Laboratory.