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 in support of the National Homeland Security Research Center, US EPA by Region 5 Chicago Regional Laboratory.

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.

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 ? g/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 ? g/L reporting limit.

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.

2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

ASTM Standards

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 in a Single Laboratory Using a Control Sample Program

Other Documents

Keywords

liquid chromatography; mass spectrometry; organophosphonates;

ICS Code

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

DOI: 10.1520/D7597-09

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