Field analysis of mercury in water, sediment and soil using static headspace analysis Page: 3 of 10
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To te 100 oiL of erctuy-dosed water in the l-L botle, 10.0 mL of a satrraxed SnC,
solution was added after which a small square (7.5 cm x2.S cm) of paraflm was rapidly
secured atop the bottle. The cap was then pressed gently over the parafllm and the botle
vigorously shaken (manually) for one minute. Ne., the cap was removed and the
para ilm seal was pncturd using the probe tip ilustraled in Figure 1. A 10-s air sample
was taken. The parafikm seal reduces the possibility of variable amounts of unequilibrated
air entering the bottle while sampling and thus increases precision of replicat
To identify the time interval necessary for establishment of equilibrium between
the aqueous phase and the headspace vapor. seven 1-L bottles containing 100.0 mL of
demonized water were dosed with 100.0 pL of a 5.0 x 104 M Hg(NOA solution. A 0.0,
mL aliquot of a saturated SnC2 solution was added to each bottle, followed by vigorous
manual agitation for 30 s for one sample, and 1.0 min for the other six samples. The
headspace vapor In the bottle equilibrated for 30 s, and the vapor in one of the bottles
agitated for 110 x~n, were analyzed immediately following agitation. The five remaining
bottles were placed on the bencbmp following the one minute agitation, until the
headspace was analyzed using the field analyzer technique at intervals of 5 min, 2 hr, 5
hr, and 22 hr. Results from the kinetic study showed that equilibrium between the
aqueous phase and the headspace vapor is reached between 30 seconds and a one minute
Environmemal water samples were collected from surface water outfalls, storm
sewers and sumps in several buildings at the U.S. Department of Energy's Y-12 Plant in
Oak Ridge, Tennessee. Additional samples were collected from the East Fork Poplar
Creek (EFPC), which oirigmales at the Y-12 Plant. The 100-mn aliquots were transferred
to 1-L polypropylene bottles for field analysis. Laboratory analyses were performed
using EPA method 245.1 (EPA, 1982).
A signal of s; 0.003 mg/n in air (coresponding to S 0.09 pg/LIn water) is
believed from experience so be spurious and therefore this value is reported as the
approximate detection limit. The upper limit for an undiluted water sample is determined
by the maximm insnumenrt reading (1.99 and0.99 mg/r? for the Jerome Model 411 and
431, respectively) and varies from about 10 to 45 pg/L depending on the model being
used. A typical relative standard deviation for replicate measurements is about 10%.
The formula converting signal to aqueous mercury concentration follows:
Signal (tog Hg/r? air) x Constant = pg Hg/L water
The constant, which should be determined using one or more aqueous standard. converts
mg/nt of ai to pgIL of water, accounts for the aqueous and vapor volumes in the
system, and adjusts for partitioning between phases according to Henry's Law. This
constant varles among, and with the condition of, each instruent (Jerome Model 411 vs.
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Kriger, A.A. & Turner, R.R. Field analysis of mercury in water, sediment and soil using static headspace analysis, article, December 31, 1994; Tennessee. (digital.library.unt.edu/ark:/67531/metadc673250/m1/3/: accessed November 16, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.