Table 1. Sample preparation, holding times, and storage conditions for VOA vial
experiments.
First experiment
Soil plugs transferred to empty VOA vial then spiked (n = 24). Samples prepared for analysis
by passing 5.00 mL of MeOH through septa.
Day 0
Day 3
Day 7
Day 14
21C
21, 4, & 12C
21, 4, & 12C
NS
(n = 3)* 3
(n = 3)* 3
(n = 3)*
(n = 3)*
Second experiment (three sets)
A. Spiked soil plug transferred to VOA containing 5 mL of water (n = 9).
B. Spiked soil plug transferred to empty VOA vial (n = 9). Samples
prepared for analysis by passing 5.00 mL of water through septa.
C. Spiked soil plug transferred to empty VOA vial (n = 9). Samples
prepared for analysis by passing 5.00 mL of MeOH through septa.
For each set.
Day 0
Day 4 or 5
Day 13 or 14
4C
12C
NS
(n = 3)*
(n = 3)†
(n = 3)*
(n = 3)*
Third experiment
Spiked soil plug transferred to empty VOA vial (n = 18). Samples prepared for analysis by
passing 5.00 mL of MeOH through septa.
For each set.
Day 0
Day 1
Day 2
Day 5
Day 7
Day 14
4C
4C
4C
12C
12C
NS
(n = 3)*
(n = 3)*
(n = 6)†
( n = 3)*
(n = 3)*
(n = 3)*
(n = 3)*
NS Not stored.
* Number of replicate analyzed after a storage period.
† Number of replicates moved from one storage condition to another, after a given period.
tablish the D0 analyte concentrations. For each of
capped. In all, three sets of samples were prepared
the sets, the six remaining samples were refriger-
in this fashion. The first set of nine was placed into
ated (4 2C) for four or five days before tripli-
22-mL VOA vials that already contained 5 mL of
cates were removed and analyzed. The remaining
organic free water. The second nine were placed
triplicates from each set were transferred to a
in empty 40-mL VOA vials. The last nine were
freezer (12 3C) and stored for an additional
placed into empty 22-mL VOA vials. In addition
nine days prior to analysis (Table 1).
to treating the soil samples, aliquots of the aque-
A third experiment was performed using only
ous spiking solution were transferred to VOA vi-
empty 40-mL VOA vials while following the same
als, three containing 5.00 mL of MeOH and six con-
sample treatment procedure as the second experi-
taining 5.00 mL of water, to establish the spiking
ment. For this experiment 18 replicates were made
solution concentration for each set. After all the
and samples were prepared for analysis by add-
samples had been prepared, either 5.00 mL of
ing 5.00 mL of MeOH to the VOA vials. Triplicates
MeOH or water was introduced to the first, fourth,
were prepared for analysis on D0, and after one,
and last of the samples contained in empty VOA
two, and five days of storage at 4 2C. In addi-
vials (no additional water was added to the 22-
tion, after two days of storage at 4 2C, six repli-
mL VOA vials that already contained water) as
cates were transferred to a freezer (12 3C). Trip-
described in the first experiment. Similarly spaced
licates of the samples placed in the freezer were
triplicates from all three sets were analyzed to es-
9
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