The behavior of the 15 analytes in this study
Connecticut River water was selected as the prin-
varied significantly, falling into four different
cipal test matrix based on the results discussed
groups. In the first group, analyte concentrations
above. The analytes were divided into four groups
appeared to be stable with or without acidifica-
as described above (Table 4). The river water was
tion over the entire 64-day period. This group in-
fortified at concentrations ranging from 50 to 150
g/L and divided into two portions. The first por-
cluded HMX and RDX (Fig. 8), and their behavior
is consistent with the results of our earlier study
tion was divided into 11 subsamples and stored in
(Grant et al. 1993) and that of Maskarinec et al.
22-mL glass vials. These samples served as con-
(1991).
trol samples to assess analyte losses without pres-
For the second group, the concentrations in the
ervation. The second portion was acidified to pH
acidified samples remained stable for at least 28
2.0 by addition of sodium bisulfate (1.5 g/L) and
days (and for all but tetryl for 64 days), but con-
was also divided into 11 subsamples. On day 0
centrations in the unacidified samples declined at
(about 416 hours after preparation), six replicates
variable rates over the entire period. This group
each of the control and preserved samples were
includes tetryl, TNB, TNT, 1,3-dinitrobenzene
analyzed to establish initial concentrations for later
(DNB), 2,6-DNT, and 2,4-DNT in decreasing order
comparison. The remaining samples of control and
of the rate of concentration decline (Table 6, Fig.
preserved water were held under refrigeration in
9). The difference in stability of these analytes for
the dark for up to 64 days. One replicate sample of
acidified and unacidified samples is clearly shown
the control and acidified water was analyzed in
in the chromatograms for fortification groups 1
triplicate on days 3, 7, 14, 28, and 64 (Table 6).
Table 6. Results of holding-time study using fortified Connecticut River water.
Concentration ( X S)
(g/L)
Preserved
Analyte
(pH 2.0)
Day 0
Day 3
Day 7
Day 14
Day 28
Day 64
64.6 1.33
66.1 0.58
67.1 0.79
65.8 1.92
66.3 0.86
63.1 0.28
HMX
No
66.2 0.83
64.3 2.85
62.2 0.94
64.2 0.86
63.3 0.34
59.5 0.48
Yes
100.5 0.9
97.1 1.0
97.0 0.6
98.9 2.9
100.5 0.7
97.0 0.38
RDX
No
102.8 1.3
100.9 1.9
97.3 0.97
100.7 0.17
99.7 1.86
97.6 0.63
Yes
41.2 0.58
10.3 0.44
11.0 0.33
tetryl
No
<d
<d
<d
40.4 0.87
41.8 0.76
42.4 0.37
41.7 0.90
41.2 0.58
32.5 5.10
Yes
52.7 1.63
29.8 0.48
17.7 0.08
7.5 0.59
0.7 0.0
TNB
No
<d
53.4 0.97
52.0 1.06
51.3 0.22
54.1 0.63
51.8 0.23
45.9 2.72
Yes
91.4 0.37
75.4 1.24
65.9 0.36
50.8 3.42
32.7 0.31
13.4 0.45
TNT
No
92.9 2.04
91.0 1.75
89.3 2.52
95.4 0.70
90.4 1.18
89.6 0.12
Yes
39.9 0.52
37.2 0.32
33.3 0.11
28.5 0.17
23.8 0.38
11.3 0.25
DNB
No
39.9 0.58
39.8 0.29
39.0 0.76
39.1 0.20
39.0 0.18
38.5 0.37
Yes
99.2 1.34
96.2 1.38
90.7 0.60
84.4 1.38
84.9 0.82
73.5 0.88
2,6-DNT
No
97.2 2.14
95.9 0.53
91.9 0.31
94.8 0.43
94.6 0.46
94.3 1.02
Yes
69.7 0.38
68.8 0.15
68.3 0.04
66.1 4.73
63.7 0.27
58.8 0.38
2,4-DNT
No
69.9 0.59
68.6 0.51
67.2 0.48
71.5 1.07
67.3 0.44
66.1 0.05
Yes
57.2 0.42
57.5 0.09
55.3 0.23
54.0 2.39
54.0 0.80
50.4 0.30
4ADNT
No
57.4 1.50
46.4 1.16
44.3 0.38
43.1 2.16
43.8 0.25
41.4 0.13
Yes
59.5 0.32
54.4 0.37
48.4 0.16
45.9 0.05
40.0 0.44
30.9 0.31
3,5-DNA
No
58.2 0.15
53.3 2.29
52.1 0.49
52.7 0.84
51.8 0.21
51.3 0.11
Yes
79.5 1.03
77.0 0.68
73.1 0.89
73.4 0.49
69.0 0.53
62.9 0.30
2ADNT
No
77.8 0.43
73.4 2.38
71.1 0.38
73.0 0.72
71.5 0.41
70.8 0.36
Yes
74.4 0.69
71.2 1.18
65.6 0.79
64.1 5.47
61.1 0.57
53.7 1.06
2NT
No
74.1 1.01
68.4 0.55
63.5 0.98
68.7 0.76
60.9 1.13
49.5 4.35
Yes
59.9 1.95
54.4 0.44
51.3 0.24
49.5 0.41
46.4 1.10
40.9 0.61
3NT
No
60.1 1.07
53.8 0.07
50.5 0.64
48.6 1.32
45.6 1.06
40.4 1.35
Yes
178.4 1.0
163.2 2.5
153.3 0.9
150.2 0.3
136.3 4.6
129.7 0.9
4NT
No
176.5 1.7
161.6 4.8
150.4 0.78
149.0 0.50
138.6 0.69
126.8 2.61
Yes
43.6 0.48
42.4 0.62
40.6 0.25
40.8 0.45
40.3 0.35
37.7 0.53
NB
No
43.2 1.46
41.2 0.58
40.2 0.86
40.6 0.27
39.6 0.90
37.9 0.64
Yes
* X = mean; S = standard deviation
12