tion in the spiked sample of 0.0045 g/g. The jars
ation samples prepared as described above and
were capped and stored at room temperature in
stored in 120-mL jars, the analyst added water and
the dark. Samples were taken from analysis on
solvent directly to the sample. For those samples
days 0, 14, 28, and 76.
stored in ampoules, the ampoule was placed into
Procedures that failed to produce stable con-
a 120-mL jar containing solvent and water, the jar
centrations in spiked samples include the follow-
was capped, and then it was shaken to break the
ing (all samples were stored at room temperature
ampoule (Hewitt 1994). For those samples stored
in the dark):
in 22-mL vials, the cap was removed from the vial
1. Repetitive additions of an aqueous solution
and the vial placed upside-down in a 120-mL jar
of white phosphorus to wet soil (AEC Standard)
containing water and solvent.
in 120-mL jars.
Samples were shaken for 18 hr, then white phos-
2. Spiking wet soil (AEC Standard) with an
phorus was determined in the soil extracts using
aqueous solution of white phosphorus in am-
a gas chromatograph equipped with the nitrogen-
poules and flame sealing.
phosphorus detector. High concentration samples
3. Incubation of wet soil (AEC Standard) with
had to be diluted by a factor of 1:10,000 to be within
a large piece (12 g) of solid white phosphorus, re-
the linear calibration range.
moval of the piece of white phosphorus, then dis-
pensing of soil into ampoules and 22-mL vials.
4. Spiking of wet soil (AEC Standard) in am-
RESULTS AND DISCUSSION
white phosphorus dissolved in mineral oil.
High concentration performance evaluation
5. Spiking of wet sand (U.S. Silica) in 22-mL vi-
samples
als with white phosphorus dissolved in mineral
Wet soils spiked with particles of white phos-
oil.
phorus were stable for greater than 100 days after
storage at room temperature in the dark (Fig. 1).
After 200 days, some samples appeared to have
Analysis
Samples were analyzed using SW-846 Method
slightly lower concentrations (Fig. 1). Linear re-
7580 (U. S. EPA 1995). For this method, water is
gression of white phosphorus concentration vs.
time gives a slope of 0.057 [concentration (g/
added to each soil/sediment sample to form a
slurry, then the white phosphorus is extracted with
g)/day] with 95% confidence limits of 0.011 and
isooctane by vigorous shaking. Each sample is
0.104. After 288 days, the loss was only 6%. This
shaken in a 120-mL jar. For the performance evalu-
apparent loss may be due to a systematic error or
300
200
100
0
100
200
300
Time (day)
Figure 1. Concentration found in wet soil samples spiked with par-
ticulate white phosphorus and stored at room temperature in sealed
120-mL jars.
3
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