Table 8. Average and standard deviations (n = 3) of analyte concentrations (g/kg) for the
sample spike and samples after various holding periods in VOA vials under different stor-
age conditions. From D0 to D5 or D4 at 4 2C, and from D5 or D4 to D14 or D13 at 12 3C.
Procd./Store*
TDCE
CDCE
Ben
TCE
Tol
PCE
E-Ben
p-Xyl
o-Xyl
A. Soil added to water in VOA vial
361
471
221
541
291
391
301
281
311
Spike
291
361
171
413
191
253
152
131
141
D0
193
203
101
303
8.51
202
5.91
3.81
9.81
D5
65%†
55%
59%
73%
45%
80%
39%
29%
70%
161
171
8.91
282
7.11
192
5.51
3.31
9.41
D14
55%*
47%
52%
68%
37%
76%
37%
25%
67%
B. Water added to soil in VOA vial
351
452
211
521
281
382
301
281
321
Spike
281
351
171
401
191
271
171
141
161
D0
181
191
111
311
9.11
231
6.81
4.31
111
D4
64%
54%
65%
78%
48%
85%
40%
30%
69%
141
162
9.41
261
7.61
201
5.41
3.51
8.61
D13
50%*
46%
55%
65%
40%
74%
32%
25%
54%
C. MeOH added to soil in VOA vial
401
491
231
561
291
401
321
302
342
Spike
383
473
221
523
311
412
291
261
341
D0
301
272
131
471
131
361
141
121
262
D5
79%
57%
59%
90%
42%
87%
48%
46%
76%
272
283
111
471
121
372
132
102
262
D14
71%
60%
50%
90%
39%
90%
45%
38%
76%
*Sample preparation procedure and storage times.
†Percent recovery relative to D0 sample concentration.
Although not reported here, preliminary experi-
tions is necessary, few Department of Transporta-
ments have been performed to investigate the ap-
tion (DOT) regulatory requirements must be met,
pearance of acetone in soil samples preserved with
and field personnel don't have to handle chemi-
sodium bisulfate. Consistent with earlier reports,
cals or weigh samples. The first and last advan-
acetone was detected in freshly collected CRREL
tages listed above go hand-in-hand, and allow
soils (5 g) preserved with sodium bisulfate (1 g),
samplers to perform sample collection and track-
while it was not found in collocated samples that
ing in a fashion that is similar to what was per-
were not acidified. Furthermore, with the excep-
formed under the guidance from Method 5030.
tion of Ottawa sand, acetone was found when
The amount of training to cover the change from
analyzing soils that had been air-dried and sieved
spatulas to modified syringes or En Core samplers
in preparation for laboratory studies. In the case
would be easily addressed in comparison to that
of the laboratory soils, acetone was found in both
which would be necessary to establish and super-
acidified and nonacidified samples; however, there
vise protocols for the handling of MeOH and acidi-
was a two-fold greater concentration of acetone
fied aqueous solutions. Moreover, preservation by
in the acidified samples. Greater concentrations
acidification cannot be used indiscriminately; that
of acetone in laboratory soils and its appearance
is, this technique cannot be used with carbon-
in-field soils was found to be associated with both
aceous soils or when styrene is a VOC of interest
lowering the pH and presence of sodium. While
(Hewitt 1995a). An additional concern is that by
not conclusive, the source of acetone is likely to
lowering the pH (with sodium bisulfate) of some
be the decomposition of natural biologically pro-
matrices, the formation of acetone, a regulated
duced compounds in either low pH or reduced
compound itself, has been observed*.
moisture conditions.
When storage at 12 3C is used as the method
of sample preservation, two or three collocated
*Personal communication, Daksha Dalal, USACE, Kan-
samples could be collected, transported, and
sas City District, 1998, and several others.
16
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