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National Water Quality Laboratory

Friday December 15, 2017

USGS Water-Resources Investigations Report 01-4132

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory — Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water with Cold Vapor-Atomic Fluorescence Spectrometry

John R. Garbarino and Donna L. Damrau

2001

An analytical method using cold vapor-atomic fluorescence spectrometry was developed by the U.S. Geological Survey in 2001 for the determination of organic plus inorganic mercury in filtered and unfiltered natural water. This method was developed to eliminate the use of acid dichromate preservative and to provide capability to measure ambient mercury concentrations in natural water. Dissolved mercury includes all oxidizable mercury species present in natural water that has been filtered through a 0.45-micrometer pore size capsule filter. Whole-water recoverable mercury includes dissolved mercury species and mercury species adsorbed to particulate matter in unfiltered natural water. Mercury species can include elemental mercury, mercury (II), mercury (II) complexes, various alkyl- and phenyl-mercury compounds, and other forms of mercury. In this method, samples are collected and processed according to standard U.S. Geological Survey protocols. Samples are preserved onsite with 6N hydrochloric acid in a ratio of 1 to 100 in a borosilicate-glass bottle with fluoropolymer-lined cap. Mercury species are oxidized to mercury (II) by using bromine monochioride; excess oxidation reagent is neutralized with hydroxylamine hydrochloride. Elemental mercury produced after adding stannous chloride is purged from the solution with ultrapure argon gas into a cell in which the mercury concentration is measured by atomic fluorescence emission at 253.7 nanometers. The analytical response is linear up to 125 nanograms per liter (ng/L) of mercury, and the short-term method detection limit is about 5 ng/L. The analytical variability at 50 ng/L is about 10 percent.

This report describes the method and compares the use of hydrochloric acid to acid dichromate as a field preservative. Ambient mercury concentrations in hydrochloric acid-preserved samples stored in borosilicate-glass bottles with fluoropolymer-lined caps are shown to be stable for at least 30 days. Mercury concentrations are stable for at least 5 months after bromine monochloride is added to the sample bottles in the laboratory. The long-term average percent recoveries at 20, 45, and 75 ng/L in reagent water, filtered and unfiltered ground water, and filtered and unfiltered surface water range from 89 to 108, 96 to 103, and 94 to 98 percent, respectively.

VIEW the report. (pdf)


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