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Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Hydrogen Dimethylamidophosphate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Water by Liquid Chromatography/Tandem Mass Spectrometry
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.
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
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