Methods for the preparation and analysis of solids and suspended solids for total mercury

Techniques and Methods 5-A8
By: , and 

Links

Abstract

The methods documented in this report are utilized by the Wisconsin District Mercury Lab for analysis of total mercury in solids (soils and sediments) and suspended solids (isolated on filters). Separate procedures are required for the different sample types. For solids, samples are prepared by room-temperature acid digestion and oxidation with aqua regia. The samples are brought up to volume with a 5 percent bromine monochloride solution to ensure complete oxidation and heated at 50C in an oven overnight. Samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. A method detection limit of 0.3 ng of mercury per digestion bomb was established using multiple analyses of an environmental sample. Based on the range of masses processed, the minimum sample reporting limit varies from 0.6 ng/g to 6 ng/g. Suspended solids samples are oxidized with a 5 percent bromine monochloride solution and held at 50?C in an oven for 5 days. The samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. Using a certified reference material as a surrogate for an environmental sample, a method detection limit of 0.059 ng of mercury per filter was established. The minimum sample reporting limit varies from 0.059 ng/L to 1.18 ng/L, depending on the volume of water filtered.

Publication type Report
Publication Subtype USGS Numbered Series
Title Methods for the preparation and analysis of solids and suspended solids for total mercury
Series title Techniques and Methods
Series number 5-A8
DOI 10.3133/tm5A8
Year Published 2004
Language English
Publisher U.S. Geological Survey
Contributing office(s) Toxic Substances Hydrology Program
Description 23 p.
Larger Work Type Report
Larger Work Subtype USGS Numbered Series
Larger Work Title Book 5. Laboratory Analysis, Section A. Water Analysis
Google Analytic Metrics Metrics page
Additional publication details