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
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
- Статус документа:
- Действующий
- Формат:
- Электронный (PDF)
- Количество страниц:
- 13
- Дата публикации:
- 15 июня 2017 г.
- Издание:
- D7597
- ICS:
- 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 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 test method has been investigated for use with reagent and surface water. 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 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 ...
Abstract
Overview
ASTM D7597-16(2017) is an international standard developed by ASTM International for the determination of specific organophosphonate compounds in water. The method utilizes liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS) using electrospray ionization (ESI) to identify and quantify trace levels of degradation products from organophosphorus chemical agents. These compounds include diisopropyl methylphosphonate (DIMP), ethyl hydrogen dimethylamidophosphate (EHDMAP), ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic acid (IMPA), methylphosphonic acid (MPA), and pinacolyl methylphosphonic acid (PMPA).
Designed to support environmental monitoring and water analysis efforts, this standard is applicable to both surface and reagent water and is significant for laboratories engaged in the detection of chemical warfare agent degradation products.
Key Topics
- Target Compounds: Focus on six specific organophosphonate analytes associated with the degradation of chemical warfare agents such as Sarin (GB), Soman (GD), Tabun (GA), and VX.
- Analytical Methodology: Involves direct injection of water samples followed by LC/MS/MS analysis using single reaction monitoring (SRM) to achieve both qualitative and quantitative results.
- Detection and Reporting: Establishes detection verification levels (DVLs) and reporting ranges for each analyte, ensuring sensitivity and reliability across various sample types.
- Quality Control: Places strong emphasis on laboratory quality assurance, including method blanks, laboratory control samples (LCS), matrix spikes, and surrogate recoveries to validate accuracy and precision.
- Interference Management: Addresses potential analytical interferences from sample matrices, solvents, reagents, and glassware. Recommends stringent contamination control and cleanliness procedures for accurate readings.
- Instrument Calibration: Details calibration procedures using multiple concentration levels and linear or quadratic regression to ensure instrument performance and data validity.
- Regulatory Alignment: Developed to align with internationally recognized standardization principles such as those set by the WTO TBT Committee.
Applications
- Water Quality Monitoring: Essential for environmental laboratories, regulatory agencies, and industry professionals monitoring surface and drinking water for organophosphonate contaminants resulting from chemical agent degradation.
- Public Health Protection: Supports early detection and quantification of hazardous organophosphonate compounds, thus helping mitigate risks to public health from potential water contamination.
- Defense and Security: Facilitates the surveillance of water sources for remnants of nerve agents and promotes compliance with chemical weapons demilitarization and nonproliferation efforts.
- Research and Development: Provides a validated approach for academic and governmental research laboratories focused on the environmental fate and behavior of organophosphate and organophosphonate compounds.
Related Standards
- ASTM D1129: Terminology Relating to Water
- ASTM D1193: Specification for Reagent Water
- ASTM D2777: Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
- ASTM D3694: Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
- ASTM D5847: Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
- ASTM D3856: Guide for Management Systems in Laboratories Engaged in Analysis of Water
- ASTM E2554: Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
These related standards provide essential guidance for terminology, calibration, sample preparation, quality management, and analytical precision within the scope of water analysis.
By following ASTM D7597-16(2017), laboratories can ensure standardized, reliable, and sensitive detection of organophosphonate analytes in water, supporting regulatory compliance and the protection of public and environmental health.
Технические детали
- Технический комитет
- D19 - Water
- SKU
- ASTM D7597-16(2017)
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