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ASTM International - ASTM D7597-16

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

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Organization: ASTM International
Publication Date: 1 February 2016
Status: inactive
Page Count: 13
ICS Code (Examination of water for chemical substances): 13.060.50
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... View More

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 (%)

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.

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

Document History

June 15, 2017
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...
ASTM D7597-16
February 1, 2016
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...
December 1, 2009
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 Chro
1.1 This procedure covers the determination of diisopropyl methylphosphonate (DIMP), ethyl hydrogen dimethylamidophosphate (EHDMAP), ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic...
December 1, 2009
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 Chro
1.1 This procedure covers the determination of diisopropyl methylphosphonate (DIMP), ethyl hydrogen dimethylamidophosphate (EHDMAP), ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic...
December 1, 2009
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 Chro
1.1 This procedure covers the determination of diisopropyl methylphosphonate (DIMP), ethyl hydrogen dimethylamidophosphate (EHDMAP), ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic...
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