1.1This 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.
1.2This test method has been developed by US EPA Region 5 Chicago Regional Laboratory (CRL).
1.3The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4The detection verification level (DVL) and reporting range for the organophosphonates are listed in Table 1.
1.4.1The 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 |
1.5This 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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