1.5 cm3) with each push. Samples were co-located by
dispersed, then allowed to sit overnight before aliquots
making these pushes at diagonal corners of a small
of the extract were decanted off. Up to three separate
square (3.8 3.8 cm). Therefore, subsamples from two
aliquots of the MeOH extract were removed from each
diagonal corners were composited for on-site analysis,
VOA vial by pouring a portion of the clear solvent layer
and the other two corners were composited for off-site
directly into small 1.9-mL vials. A complete set of these
analysis. To transfer the prescribed weight of soil, the
MeOH extracts, including two trip blanks (VOA vials
syringe was tared before use and then weighed again
containing only MeOH and the surrogates compounds),
after collection. The samples were adjusted to ensure
was sent to the reference laboratory and also returned
that each weighed 5.0 0.2 g by slightly over-filling
to CRREL for analysis, and several sample aliquots and
(more than 5 g), then shaving excess soil off the end
two trip blanks were sent to the QA laboratory.
with a spatula, to attain the desired weight. Once it was
obtained, the 5.0 0.2-g sample was immediately
GRO compounds in water
extruded into a VOA vial that contained 10 mL of
For aqueous matrices contaminated with GRO com-
extraction solvent.
pounds, 16 bulk water samples (Table 1) were obtained
To take sample duplicates, the same location in the
from within the gasoline contaminant plume by com-
plastic core barrel liner was sampled by pushing the
pletely filling either a 1- or 4-L amber glass bottle. The
modified syringe to a greater depth in each of the four
larger sized bottle was only used when the volume nec-
corners of the square. As above, samples from diago-
essary for the sample duplicate was collected. Soon after
nal corners were obtained by pushing the syringe into
these bottles were delivered to the sample distribution
soil surface twice, before the weight was adjusted and
trailer, they were gently swirled. Then two to four VOA
the sample extruded into the prepared VOA vials.
vials were completely filled and capped, and a 500-mL
The soil matrix blank was initially obtained from a
aliquot was slowly decanted into a separatory funnel
core barrel liner as a bulk sample by transferring about
(two in the case of the sample duplicate).
300 g to a 250-mL bottle. This background sample was
Matrix blank samples were prepared by decanting
obtained 2 days before the technology demonstration
water directly from one of the plastic jugs filled with
began. The same modified syringe was used to obtain
background water into 40-mL VOA vials or into a
5.0 0.2 g of soil from this bottle. These matrix blank
separatory funnel. Matrix spike samples were prepared
samples were then transferred to a VOA vial contain-
by filling four 1-L bottles with 1050 mL of the back-
ing 10 mL of solvent. This same process was used when
ground water, then spiking (Table 2). These matrix spike
the matrix spike samples (Table 2) were prepared,
samples were prepared 1 day prior to use, and were
except that an aliquot of a commercial standard was
stored in a refrigerator. Subsamples were decanted from
added.
these bottles in the same way used for the discrete
Performance evaluation samples for GRO com-
groundwater samples. Four PE samples were prepared
pounds were prepared by spiking soil (silty clay) that
by spiking 1.00 L of HPLC grade water, held in four
had been sieved, autoclaved, and air dried in a class
separate 1-L glass bottles (Table 3). These samples were
100 clean air station (Table 3). For these samples, 5.00
also prepared and distributed using the same procedure
0.02 g of soil was transferred to a 5-mL glass
as used for the discrete groundwater samples.
ampoule at CRREL, then shipped to the site where it
Immediately after a water sample was decanted into
was immediately sealed with a propane torch after spik-
a separatory funnel, it was returned to the technology
ing, 2 days prior to the start of the technology demon-
developer for extraction. A complete set of the water
stration. These samples were stored in a freezer until
samples contained in the 40-mL VOA vials was sent to
they were used. In preparation for analysis, a sealed
the reference laboratory and also to CRREL for analysis,
ampoule was placed inside of a VOA vial containing
and a few VOA vials were sent to the QA laboratory.
10 mL of solvent, the VOA vial was capped, and the
DRO compounds in soil
ampoule was broken open and its contents completely
dispersed by shaking. Several brief episodes of manual
For soil samples contaminated with DRO/bunker
shaking were necessary to ensure that all of the soil was
C, the test plan specified that 27 samples be distributed
dispersed into the solvent phase.The presence of broken
for analysis (Table 1). After the core barrel liners were
glass in these sample vials allowed them to be distin-
opened as described before, bulk soil samples of about
guished from the others that were analyzed on-site.
200 g were removed from the depths of interest using a
All of the soil samples placed into the VOA vials
stainless steel spatula and placed into a 250-mL glass
for on-site analysis were delivered to the technology
bottle. The contents of the bottle were then briefly
developer within 1 hour. Soil samples placed into the
homogenized (mixed) with a spatula. After mixing, two
VOA vials containing 10 mL of MeOH were initially
different plastic syringe sampling tools were used to
6
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