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Description of ASTM-D7597 2017ASTM D7597-16-Reapproved2017Active Standard: 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 SpectrometryASTM D7597Scope 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
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)
TABLE 3 Multi-Laboratory Recovery Data in Reagent Water
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. 1.6 This 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. Keywords liquid chromatography; mass spectrometry; organophosphonates; ICS Code ICS Number Code 13.060.50 (Examination of water for chemical substances) DOI: 10.1520/D7597-16R17 This book also exists in the following packages...Subscription InformationMADCAD.com ASTM Standards subscriptions are annual and access is unlimited concurrency based (number of people that can access the subscription at any given time) from single office location. For pricing on multiple office location ASTM Standards Subscriptions, please contact us at info@madcad.com or +1 800.798.9296.
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About ASTMASTM International, formerly known as the American Society for Testing and Materials (ASTM), is a globally recognized leader in the development and delivery of international voluntary consensus standards. Today, some 12,000 ASTM standards are used around the world to improve product quality, enhance safety, facilitate market access and trade, and build consumer confidence. ASTM’s leadership in international standards development is driven by the contributions of its members: more than 30,000 of the world’s top technical experts and business professionals representing 150 countries. Working in an open and transparent process and using ASTM’s advanced electronic infrastructure, ASTM members deliver the test methods, specifications, guides, and practices that support industries and governments worldwide. |
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