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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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 test method. This test method adheres to single reaction monitoring (SRM) mass spectrometry.

1.2 This test method has been developed by U.S. 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.

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

1.4.1 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.

FIG. 1 Example ESI Positive Mode SRM Chromatograms Signal/Noise Ratios

FIG. 2 Example ESI Negative Mode SRM Chromatograms Signal/Noise Ratios

1.4.2 The 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

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Published:: 06/15/2017
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ASTM D7597-16(2017) PDF

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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ASTM D7597-16(2024)

ASTM D7597-16(2017)

ASTM D7597-16

ASTM D7597-09e2

ASTM D7597-09e1

ASTM D7597-09

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