ASTM D 7597 : 2016 : R2017
Superseded
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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
Hardcopy , PDF
20-05-2024
English
13-07-2017
CONTAINED IN VOL. 11.02, 2018 Defines 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).
| Committee |
D 19
|
| DocumentType |
Test Method
|
| Pages |
13
|
| ProductNote |
Reconfirmed 2017
|
| PublisherName |
American Society for Testing and Materials
|
| Status |
Superseded
|
| SupersededBy | |
| Supersedes |
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 test method. This test method adheres to single reaction monitoring (SRM) mass spectrometry.
1.2This test method has been developed by U.S. 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.
TABLE 1 Detection Verification Level and Reporting Range
| Analyte | ESI Mode | DVL (μg/L) | Reporting Range (μg/L) |
| Diisopropyl methylphosphonate | Positive | 1 | 5–150 |
| Ethyl hydrogen dimethylamidophosphate | Negative | 0.25 | 5–150 |
| Ethyl hydrogen dimethylamidophosphate | Positive | 0.25 | 5–150 |
| Ethyl methylphosphonic acid | Negative | 5 | 50–1500 |
| Ethyl methylphosphonic acid | Positive | 5 | 50–1500 |
| Isopropyl methylphosphonic acid | Negative | 10 | 50–1500 |
| Isopropyl Methylphosphonic acid | Positive | 5 | 50–1500 |
| Methylphosphonic acid | Negative | 20 | 100–1500 |
| Methylphosphonic acid | Positive | 10 | 50–1500 |
| Pinacolyl methylphosphonic acid | Negative | 5 | 50–1500 |
| Pinacolyl methylphosphonic acid | Positive | 5 | 50–1500 |
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.
FIG. 1Example ESI Positive Mode SRM Chromatograms Signal/Noise Ratios
FIG. 2Example ESI Negative Mode SRM Chromatograms Signal/Noise Ratios
1.4.2The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the organophosphonates except for MPA in the ESI negative mode which is at Level 2 due to not meeting the DVL criteria at the lower concentration level. The DVL for MPA in the ESI negative mode is at 20 μg/L, which forces a raised reporting limit. However, the multi-laboratory validation required a spike of all target analytes at Level 1 concentrations. The mean recovery for MPA in the ESI negative mode at this level was 98.7 % as shown in Table 3. If your instrument’s sensitivity can meet the requirements in this test method, MPA may have a 50 μg/L reporting limit.
TABLE 2 Concentrations of Calibration Standards (PPB)
| Analyte/Surrogate | LV 1 | LV 2 | LV 3 | LV 4 | LV 5 | LV 6 | LV 7 |
| Diisopropyl methylphosphonate | 5 | 10 | 20 | 35 | 50 | 100 | 150 |
| Ethyl hydrogen dimethylamidophosphate | 5 | 10 | 20 | 35 | 50 | 100 | 150 |
| Ethyl methylphosphonic acid | 50 | 100 | 200 | 350 | 500 | 1000 | 1500 |
| Isopropyl methylphosphonic acid | 50 | 100 | 200 | 350 | 500 | 1000 | 1500 |
| Methylphosphonic acid | 50 | 100 | 200 | 350 | 500 | 1000 | 1500 |
| Pinacolyl methylphosphonic acid | 50 | 100 | 200 | 350 | 500 | 1000 | 1500 |
| DIMP-D14 (Surrogate) | 5 | 10 | 20 | 35 | 50 | 100 | 150 |
| PMPA-13C4 (Surrogate) | 25 | 50 | 100 | 175 | 250 | 500 | 750 |
| MPA-D3 (Surrogate) | 25 | 50 | 100 | 175 | 250 | 500 | 750 |
TABLE 3 Multi-Laboratory Recovery Data in Reagent Water
| Analyte | ESI | Spike Conc. | # Results | # Labs | Bias | Precision | |||||
| Mean | Min | Max | Overall SD | Pooled | Overall | Pooled | |||||
| 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.
1.6This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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