| ASTM D7597-16 - 1.2.2016 | |||||||||||
| Significance and Use | |||||||||||
5.1 Organophosphate pesticides affect the nervous system by disrupting the enzyme that regulates acetylcholine, a neurotransmitter. They were developed during the early 19th century, but their effects on insects, which are similar to their effects on humans, were discovered in 1932. Some are poisonous and were used as chemical weapon agents. Organophosphate pesticides are usually not persistent in the environment.4, 5 5.2 This test method is for the analysis of selected organophosphorous-based chemical weapon agent degradation products from Sarin (GB), Soman (GD), Tabun (GA) and VX. This method has been investigated for use with reagent and surface water. | |||||||||||
| 1. Scope | |||||||||||
1.1 This procedure covers the determination of diisopropyl methylphosphonate (DIMP), ethyl hydrogen dimethylamidophosphate (EHDMAP), ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic acid (IMPA), methylphosphonic acid (MPA) and pinacolyl methylphosphonic acid (PMPA) (referred to collectively as organophosphonates in this test method) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS) using electrospray ionization (ESI). These analytes are qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry. 1.2 This test method has been developed by US EPA Region 5 Chicago Regional Laboratory (CRL). 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4 The detection verification level (DVL) and reporting range for the organophosphonates are listed in Table 1. 1.4.1 The DVL is required to be at a concentration at least three times below the reporting limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios at the DVLs for the organophosphonates in the ESI positive mode and Fig. 2 in the ESI negative mode. RSD (%) | |||||||||||
DIMP |
Pos |
5 |
16 |
4 |
95.1 |
65.8 |
136.0 |
17.6 |
19.4 |
21.3 |
22.4 |
DIMP |
Pos |
10 |
19 |
5 |
98.2 |
80.0 |
121.0 |
6.1 |
5.5 |
13.6 |
13.8 |
DIMP |
Pos |
25 |
26 |
6 |
102.9 |
74.4 |
128.0 |
5.6 |
5.7 |
14.5 |
14.1 |
DIMP |
Pos |
125 |
22 |
5 |
96.6 |
80.4 |
120.0 |
4.4 |
4.5 |
11.0 |
11.4 |
DIMP-D14 |
Pos |
25 |
86 |
6 |
102.6 |
54.8 |
127.6 |
9.8 |
9.5 |
11.2 |
10.9 |
EHDMAP |
Neg |
5 |
12 |
3 |
57.5 |
0.0 |
220.0 |
31.4 |
22.3 |
71.1 |
123.6 |
EHDMAP |
Neg |
10 |
16 |
4 |
47.1 |
0.0 |
178.0 |
13.3 |
10.8 |
66.8 |
142.0 |
EHDMAP |
Neg |
25 |
22 |
5 |
84.1 |
54.0 |
141.2 |
6.9 |
6.6 |
22.9 |
27.3 |
EHDMAP |
Neg |
125 |
18 |
4 |
87.4 |
64.2 |
141.6 |
5.0 |
5.1 |
25.4 |
29.1 |
EHDMAP |
Pos |
5 |
16 |
4 |
77.0 |
0.0 |
134.2 |
7.4 |
8.0 |
51.4 |
66.8 |
EHDMAP |
Pos |
10 |
20 |
5 |
70.0 |
0.0 |
143.0 |
7.7 |
10.0 |
53.6 |
76.5 |
EHDMAP |
Pos |
25 |
26 |
6 |
89.6 |
60.0 |
128.8 |
5.2 |
6.2 |
23.5 |
26.2 |
EHDMAP |
Pos |
125 |
22 |
5 |
87.5 |
59.0 |
123.2 |
5.2 |
6.0 |
23.9 |
27.3 |
EMPA |
Neg |
50 |
16 |
4 |
110.1 |
74.8 |
170.6 |
22.4 |
17.2 |
25.6 |
23.3 |
EMPA |
Neg |
100 |
20 |
5 |
108.3 |
87.7 |
175.0 |
11.1 |
8.7 |
24.8 |
22.9 |
EMPA |
Neg |
250 |
26 |
6 |
104.8 |
82.0 |
122.6 |
6.1 |
5.5 |
11.8 |
11.3 |
EMPA |
Neg |
1250 |
22 |
5 |
101.5 |
87.2 |
126.4 |
8.4 |
8.1 |
11.2 |
11.0 |
EMPA |
Pos |
50 |
16 |
4 |
95.4 |
77.6 |
122.8 |
12.9 |
13.3 |
13.1 |
13.7 |
EMPA |
Pos |
100 |
20 |
5 |
96.0 |
61.4 |
132.5 |
9.5 |
9.5 |
15.9 |
16.6 |
EMPA |
Pos |
250 |
26 |
6 |
99.7 |
70.0 |
133.2 |
5.9 |
5.4 |
18.2 |
18.2 |
EMPA |
Pos |
1250 |
21 |
5 |
93.9 |
84.0 |
108.4 |
2.7 |
3.0 |
7.7 |
8.2 |
IMPA |
Neg |
50 |
16 |
4 |
88.0 |
56.6 |
140.4 |
23.7 |
26.0 |
23.5 |
26.7 |
IMPA |
Neg |
100 |
20 |
5 |
88.0 |
68.5 |
118.0 |
12.9 |
14.3 |
13.4 |
15.2 |
IMPA |
Neg |
250 |
26 |
6 |
98.1 |
72.8 |
144.0 |
13.1 |
11.9 |
19.2 |
19.6 |
IMPA |
Neg |
1250 |
21 |
5 |
90.7 |
73.1 |
103.0 |
5.5 |
6.1 |
8.7 |
9.6 |
IMPA |
Pos |
50 |
16 |
4 |
98.3 |
47.8 |
139.6 |
19.2 |
20.5 |
27.2 |
27.7 |
IMPA |
Pos |
100 |
19 |
5 |
95.4 |
72.3 |
120.5 |
9.8 |
10.3 |
12.4 |
13.0 |
IMPA |
Pos |
250 |
26 |
6 |
97.0 |
79.2 |
188.4 |
7.4 |
7.6 |
10.9 |
11.2 |
IMPA |
Pos |
1250 |
21 |
5 |
91.3 |
70.4 |
115.5 |
5.1 |
5.2 |
11.4 |
12.5 |
MPA |
Neg |
50 |
16 |
4 |
98.7 |
3.3 |
175.0 |
14.2 |
25.3 |
60.5 |
61.3 |
MPA |
Neg |
100 |
20 |
5 |
100.0 |
41.9 |
142.0 |
8.9 |
9.2 |
30.8 |
30.8 |
MPA |
Neg |
250 |
26 |
6 |
99.5 |
66.0 |
124.5 |
7.6 |
7.6 |
14.5 |
14.5 |
MPA |
Neg |
1250 |
22 |
5 |
102.7 |
81.8 |
130.5 |
10.5 |
9.9 |
12.4 |
12.1 |
MPA |
Pos |
50 |
16 |
4 |
68.3 |
9.8 |
139.6 |
13.4 |
20.3 |
36.6 |
53.6 |
MPA |
Pos |
100 |
20 |
5 |
80.5 |
48.4 |
149.7 |
14.0 |
12.6 |
26.8 |
33.3 |
MPA |
Pos |
250 |
26 |
6 |
91.7 |
33.9 |
153.7 |
8.0 |
7.8 |
31.8 |
34.7 |
MPA |
Pos |
1250 |
22 |
5 |
95.8 |
31.8 |
208.2 |
12.6 |
8.3 |
43.4 |
45.3 |
MPA-D3 |
Neg |
250 |
84 |
6 |
111.2 |
57.2 |
190.8 |
16.2 |
12.5 |
30.0 |
26.9 |
MPA-D3 |
Pos |
250 |
68 |
5 |
104.4 |
58.4 |
151.8 |
14.3 |
14.0 |
18.0 |
17.3 |
PMPA |
Neg |
50 |
15 |
4 |
87.8 |
77.6 |
124.4 |
8.4 |
8.2 |
13.8 |
15.7 |
PMPA |
Neg |
100 |
19 |
5 |
91.6 |
83.6 |
98.2 |
2.8 |
3.0 |
4.4 |
4.8 |
PMPA |
Neg |
250 |
26 |
6 |
101.0 |
77.2 |
123.8 |
5.0 |
4.8 |
12.1 |
12.0 |
PMPA |
Neg |
1250 |
22 |
5 |
99.2 |
84.8 |
126.5 |
4.9 |
4.8 |
12.3 |
12.4 |
PMPA |
Pos |
50 |
16 |
4 |
90.8 |
60.8 |
148.8 |
15.8 |
16.1 |
25.6 |
28.2 |
PMPA |
Pos |
100 |
15 |
4 |
95.2 |
86.8 |
114.0 |
3.8 |
4.0 |
7.9 |
8.3 |
PMPA |
Pos |
250 |
20 |
5 |
103.8 |
85.2 |
136.1 |
4.5 |
3.8 |
15.3 |
14.7 |
PMPA |
Pos |
1250 |
12 |
3 |
99.8 |
88.8 |
117.5 |
5.2 |
5.0 |
7.5 |
7.5 |
PMPA-13C6 |
Neg |
250 |
83 |
6 |
99.5 |
74.8 |
128.3 |
9.4 |
9.2 |
11.1 |
11.1 |
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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