Over four hundred vegetation samples were collected for total Hg determination as part of a biogeochemical survey in the Precambrian Shield region near Huntsville, Ontario. An objective of the survey was to obtain accurate data describing the spatial and temporal variation of Hg concentrations in vegetation. Five tree species, clubmosses, mosses, lichen and fungi were collected along three transects each 8 to 10 km long. The samples were digested using a hot H2SO4/HNO3 mixture followed by cold-vapor AAS detection. Very low detection limits (less than 1.0 ng g−1) were achieved by performing the analyses in a clean, Hg-free laboratory. The Hg concentration of coniferous needles did not vary significantly over eight weeks of the summer, but did vary significantly between first and second year growth. In all tree species examined, Hg concentrations in needles/leaves were two to three times as high (by dry weight) as that in twig tissue from the same branch. Differences in Hg content between tissues of different types and ages constituted a major source of within-site variation between plants of the same species.