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

    Active Standard ASTM D7597 | Developed by Subcommittee: D19.06

    Book of Standards Volume: 11.02


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    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

    D1129 Terminology Relating to Water

    D1193 Specification for Reagent Water

    D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water

    D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents

    D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water

    D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis

    E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques

    Other Documents

    EPA Publication SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods


    ICS Code

    ICS Number Code 13.060.50 (Examination of water for chemical substances)

    Referencing This Standard
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    DOI: 10.1520/D7597-16

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    Citation Format

    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, ASTM International, West Conshohocken, PA, 2016, www.astm.org

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