transfer samples to empty VOA vials. One or more 40-
with 1050 mL of background water, then spiking
mL VOA vials were filled to capacity (approximately
(Table 2). The high level matrix spike was prepared by
60 g) using the EasyDraw syringeTM (U.S. Oil Com-
decanting the entire contents of five ampoules filled
pany) for the off-site laboratories, and 5.0 0.2 g of
with approximately 1.0 mL of standard reference solu-
soil was placed into a VOA vial with a modified 5-mL
tion into a bottle containing 1050 mL of water. Because
syringe for on-site preparation and analysis. As described
this commercial standard was prepared in methylene
previously, the soil sample obtained in the 5-mL
chloride, which is not soluble in water, it was neces-
syringe was handled so that only 5.0 0.2 g was deliv-
sary to add 2 mL of MeOH to the low level matrix spike
ered. Soil sample duplicates were prepared by taking
bottles, and to shake them vigorously for several min-
two rounds of samples from the same bulk sample
utes, before the spike went into solution. To get the high
bottle.
level matrix spike into solution, the majority of the water
Matrix blank samples were prepared by transferring
had to be poured into a clean bottle, then 10 mL of
the above two quantities (5.0 0.2 g and approximately
MeOH was added to the methylene chloride spike in
60 g) from a bottle containing background soil. This
the presence of only about 15 mL of water. After vigor-
same soil was also used to prepare the matrix spike
ous shaking, the methylene chloride went into solution
samples (Table 2). Two reference materials, supplied
and the water that had been removed was added back
as 20.0 0.2-g quantities in a sealed glass ampoule,
to the bottle. Aliquots from each one of these bottles
were purchased to serve as the PE samples (Table 3).
were decanted into the separatory funnel, filling it to
For on-site analysis, one ampoule of each concentra-
the 500-mL mark, then the remainder (550 mL) was
tion was opened and 5.0 0.2-g quantities were trans-
sent for reference laboratory analysis.
ferred to four VOA vials. Four intact ampoules of the
RRO compounds in soil
low level certified standard and two of the high level
were sent to the reference laboratory for analysis. Prior
For the soil contaminated with RRO compounds,
to shipping these ampoules, all of the reference sample
the test plans specified that nine samples be distributed
information was removed and they were relabeled.
(Table 1). After the cap was removed from one end of
VOA vials containing 5.0 0.2 g of soil were deliv-
the brass core barrel liner, approximately 200 g of soil
ered for on-site analysis soon after preparation. A com-
was transferred to a 250-mL glass bottle and mixed with
plete set of the VOA vials that were filled to capacity
a stainless steel spatula. After mixing, subsamples were
was shipped to the reference laboratory and a few were
removed using the same procedure as used for the soil
sent to the QA laboratory. According to the protocols
samples with DRO/bunker C range contamination. For
the soil matrix spikes, either 5.0 0.2 g or 20 g of the
used by the QA and reference laboratory, only 10- or
20-g quantities, respectively, of the soil present in these
background soil was transferred to VOA vials that were
VOA vials were removed for extraction and analysis.
then spiked (Table 2). Only one matrix spike sample
Since the matrix spike and PE samples only contained
was prepared for the reference laboratory.
20 g of soil per container, the reference laboratory was
asked to analyze the entire contents of the vessel.
LABORATORY ANALYSES
DRO compounds in water
For groundwater contaminated with DRO/bunker
To eliminate variations that could potentially exist
C, the test plan specified that 18 samples be distributed
among different sources of commercial standards, a set
(Table 1). Bulk water samples were obtained in clean
of the reference standards that had been used for mak-
4-L amber glass bottles by filling them to capacity, when
ing the matrix spike samples was distributed to all of
possible. Soon after being delivered to the trailer, these
the off-site laboratories. Each laboratory was asked to
bottles were gently swirled, then water was slowly
use these reference standards to calibrate their instru-
decanted into a separatory funnel, filling it up to the
ments prior to analyzing the field and QA samples. The
500-mL volume mark. Then, one or more 1-L amber
reference laboratory was asked to use the analytical
glass bottles were filled to capacity for the off-site labo-
methods listed in Table 4, and to establish the TPH con-
ratories. For the groundwater sample duplicate, two
centration within certain hydrocarbon ranges.
separatory funnels and two 1-L amber glass bottles were
In addition to the reference laboratory, CRREL ana-
filled from a single 4-L bottle.
lyzed all of the samples contaminated with GRO com-
The matrix blank was prepared by filling a
pounds. CRREL used Methods 5021/8021 for sample
separatory funnel with 500 mL and a 1-L glass bottle to
preparation and quantification, which specify a
capacity with background water. Matrix spike samples
headspace system coupled to a gas chromatograph
were prepared by filling four 1-L amber glass bottles
equipped with a photo ionization detector. The deter-
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