containers. Discrete samples were not subsampled, but rather the entire sample was
extracted as follows. A volume of acetonitrile in mL, approximately double the mass
of the sample in grams, was added to each 4-oz jar unless the sample was too large.
For those cases the sample was transferred to an 8-oz jar and acetonitrile was added.
All jars were capped and placed on a tabletop shaker overnight. The samples were
removed from the shaker and allowed to settle for at least an hour. Each sample was
filtered through a 0.45 m Millex FH filter and placed in a 7-ml amber glass vial.
Vials were stored in a refrigerator until analyzed.
Composite soil samples were placed on sheets of aluminum foil to air dry. Dried
samples were sieved though a #10 sieve (2.00 mm). The material that passed the
sieve was ground in a Model LM2 Laboratory Ring Mill (LabTech Essa Pty. Ltd.,
Bassendean, WA, Australia) grinder for 60 seconds. After grinding, composite
samples were spread in a thin layer on clean aluminum foil. Three subsamples were
obtained for each composite sample by collecting at least 30 increments randomly
from the layer of ground soil for a mass of about 10 g. Each 10-g subsample was
extracted with 20-mL of acetonitrile in an ultrasonic bath overnight at room
temperature. After sonication, samples were removed from the bath and allowed to
settle for at least an hour. An aliquot was then removed, filtered, and placed in a 7-ml
amber vial for storage in a refrigerator.
The extracts from both the discrete and composite samples were all analyzed using
the general procedures of SW 846 Method 8330 (EPA 1994). For this analysis, an
aliquot of each sample was diluted 1 to 4 with reagent grade water. Analysis was
conducted on a modular RP-HPLC system from Thermo Finnigan composed of a
SpectraSYSTEM Model P1000 isocratic pump, a SpectraSYSTEM UV2000 dual
wavelength UV/VS absorbance detector set at 210 and 254 nm (cell path 1cm), and a
SpectraSYSTEM AS300 auto sampler. Samples were introduced by over filling a
100-L sampling loop. Separations were made on a 15 cm x 3.9 mm (4-m) NovaPak
C-8 column (Waters Chromatography Division, Milford, MA) eluted with 15:85
isopropanol/water (v/v) at 1.4 mL/min. Concentrations were estimated against
commercial multianalyte standards (Restek) from peak heights. If concentrations
exceeded 20 ppm, an aliquot of the original extract was diluted appropriately with
additional acetonitrile prior to the 1 to 4 dilution with reagent grade water.
3.4 Sample Nomenclature
All samples were named according to the following five-parts labelling system during
Phase II:
First part: sample type
S:
Soils
SW:
Surface Water
B:
Biomass (Prairie Grass and other species)
SED:
Sediment
6
DRDC Valcartier TR 2004-204
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