ASTM E2866 - 12(2016)
Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Soil by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry
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Significance and Use
5.1 This is a performance based method, and modifications are allowed to improve performance.
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this standard are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this Standard shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.
5.2 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 were 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.7,8
5.3 This test method is for the analysis of selected organophosphorous based pesticide degradation products.
5.4 This method has been investigated for use with various soils.
1. Scope
1.1 This procedure covers the determination of Diisopropyl Methylphosphonate (DIMP), Ethyl Methylphosphonic Acid (EMPA), Isopropyl Methylphosphonic Acid (IMPA), Methylphosphonic Acid (MPA) and Pinacolyl Methylphosphonic Acid (PMPA), referred to collectively as organophosphonates (OPs) in this test method, in soil. This method is based upon solvent extraction of a soil by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). OPs are qualitatively and quantitatively determined by this method.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 The Method Detection Limit2 (MDL), electrospray ionization (ESI) mode and Reporting Range3 for the OPs are listed in Table 1.
1.4 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
D653 Terminology Relating to Soil, Rock, and Contained Fluids
D1193 Specification for Reagent Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D3740 Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
ICS Code
ICS Number Code 13.080.10 (Chemical characteristics of soil)
UNSPSC Code
UNSPSC Code 11111501(Soil)
Referencing This Standard
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DOI: 10.1520/E2866-12R16
Citation Format
ASTM E2866-12(2016), Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Soil by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry, ASTM International, West Conshohocken, PA, 2016, www.astm.org
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