plosives signatures at the surface were spatially het-
the two analysis times.* To test this hypothesis, 10
erogeneous.
archived soils were extracted using the protocol used
Of the sample extracts analyzed on site and also re-
at Fort Leonard Wood, then sequentially analyzed on
the same day by both GC-TID and GC-ECD. Table 3
turned to CRREL for analysis by GC-ECD (Method
shows the concentrations (g/kg) of 2,4-DNT and TNT
8095), only those that had an extract volume of 0.3 mL
obtained by these two methods of analysis. The good
or greater could be reanalyzed. This sample volume
agreement (low median %D) for both analytes is con-
limitation was necessary because of the capabilities of
sistent with the hypothesis that the discrepancy in the
the HP auto sampler used with the HP 6890 GC-ECD.
Table 2 shows the concentrations (g/kg) obtained for
TNT values for the Fort Leonard Wood samples was
due to TNT degradation during the time between on-
2,4-DNT, TNT, 4AmDNT, and 2AmDNT by both GC-
site and laboratory analysis (seven to 10 days).
TID and GC-ECD analysis for those sample extracts
that were analyzed both on site and in our laboratory.
Umatilla Chemical Depot
Also included in this table are the median and range of
Most of the samples analyzed on site at the Umatilla
the percent differences (%D) of the field results as com-
Chemical Depot were obtained during the character-
pared to the laboratory results. This comparison shows
ization of an area that had been used for the OB/OD of
that the median percent differences for 2,4-DNT,
2AmDNT, and 4AmDNT were less than 10%. The TNT
munitions. Furthermore, prior to the analysis by GC-
TID, several of the samples had been identified as hav-
values established in the field with GC-TID, however,
were biased high. One explanation for this discrepancy
is that TNT at these low concentrations (less than 250
g/kg) was not stable in the acetone extracts, therefore
*Personal communication, Marianne E. Walsh, Chemical
Engineer, CRREL, Hanover, New Hampshire, May 2000.
the TNT concentrations may have decreased between
Table 2. Comparison between GC-TID-1 field and GC-ECD laboratory (Method 8095) results for
explosives in solvent extracts of samples collected at the Fort Leonard Wood minefield.
Analyte concentration (g/kg)
2,4-DNT
TNT
4AmDNT
2AmDNT
TID-1
ECD
TID-1
ECD
TID-1
ECD
TID-1
ECD
1.
270
240
18
9.5
350
240
320
250
2.
320
370
25
18
320
370
470
490
3. 1100
1300
220
180
2200
2500
2800
3000
4.
7.1
7.9
ND
0.8
ND*
19
44
42
5.
4.4
3.7
ND
ND
22
9.9
21
17
6.
ND
ND
ND
ND
ND
2.9
ND
3.2
7.
49
47
26
3.8
190
170
180
160
8.
26
27
12
2.5
100
100
110
96
9.
31
28
13
1.6
42
65
96
68
10.
17
21
5.4
1.2
41
31
35
38
11.
3.5
3.8
1.5
0.8
ND
8.4
7.2
10
12.
ND
0.7
ND
ND
ND
2.4
ND
3.5
13. 360
410
120
15
IF†
310
310
380
14.
110
94
9.5
1.5
170
150
350
260
Median and range of the % differences for analysis pairs (ECD reference value) with analyte concentrations.
2,4-DNT
TNT
4AmDNT
2AmDNT
Median
5.79
365
5.88
8.63
Range 19.0 to 18.9
22.2 to 712
35.4 to 122
28.0 to 41.2
*ND--Not detected
8