ASTM E2866-21

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

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.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

General Information

• Status: Published
• Publication Date: 30-Apr-2021
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Standards Content (Sample)

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.
Designation: E2866 − 21
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
1
by Liquid Chromatography/Tandem Mass Spectrometry
This standard is issued under the fixed designation E2866; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This procedure covers the determination of Diisopropyl
ization established in the Decision on Principles for the
Methylphosphonate (DIMP), Ethyl Methylphosphonic Acid
Development of International Standards, Guides and Recom-
(EMPA), Isopropyl Methylphosphonic Acid (IMPA), Methyl-
mendations issued by the World Trade Organization Technical
phosphonic Acid (MPA), and Pinacolyl Methylphosphonic
Barriers to Trade (TBT) Committee.
Acid (PMPA), referred to collectively as organophosphonates
(OPs) in this test method, in soil. This method is based upon
2. Referenced Documents
solvent extraction of a soil by pressurized fluid extraction
4
2.1 ASTM Standards:
(PFE). The extract is filtered and analyzed by liquid
D1193Specification for Reagent Water
chromatography/tandemmassspectrometry(LC/MS/MS).OPs
D2777Practice for Determination of Precision and Bias of
arequalitativelyandquantitativelydeterminedbythismethod.
Applicable Test Methods of Committee D19 on Water
1.2 Units—The values stated in SI units are to be regarded
D5681Terminology for Waste and Waste Management
asstandard.Nootherunitsofmeasurementareincludedinthis
E2554Practice for Estimating and Monitoring the Uncer-
standard.
tainty of Test Results of a Test Method Using Control
2
Chart Techniques
1.3 The method detection limit (MDL), electrospray ion-
3
ization (ESI) mode, and reporting range for the OPs are listed
2.2 Other Documents:
in Table 1.
EPApublication SW-846Test Methods for Evaluating Solid
5
Waste, Physical/Chemical Methods
1.4 This standard does not purport to address all of the
40 CFR Part 136, Appendix BThe Code of Federal Regu-
safety concerns, if any, associated with its use. It is the
6
lations
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
3. Terminology
mine the applicability of regulatory limitations prior to use.
3.1 Definitions—For definitions of terms used in this test
method, refer to Terminology D5681.
1
3.2 Definitions of Terms Specific to This Standard:
This test method is under the jurisdiction ofASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.06 on
3.2.1 analytical column, n—the particles of the solid sta-
Analytical Methods.
tionary phase fill the whole inside volume of a tube (column)
Current edition approved May 1, 2021. Published May 2021. Originally
approved in 2012. Last previous edition approved in 2016 as E2866–12 (2016).
DOI: 10.1520/E2866-21.
2 4
The MDL is determined following the Code of Federal Regulations, 40 CFR For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Part136,Appendix B utilizingsolventextractionofsoilbyPFE.Adetailedprocess contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
determining the MDL is explained in the reference and is beyond the scope of this Standards volume information, refer to the standard’s Document Summary page on
standard to be explained here. the ASTM website.
3 5
Reporting range concentrations are calculated from Table 4 concentrations Available from National Technical Information Service (NTIS), U.S. Depart-
assuming a 100 µL injection of the lowest and highest level calibration standards ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
with a 40 mL final extract volume of a 10 g soil sample. Volume variations will www.epa.gov/epawaste/hazard/testmethods/index.htm.
6
change the reporting limit and ranges. The reporting limit (RL), lowest concentra- AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
tion of the reporting range, is calculated from the concentration of the Level 1 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
calibration standard as shown in Table 4. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C7
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E2866 − 12 (Reapproved 2016) E2866 − 21
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
1
by Liquid Chromatography/Tandem Mass Spectrometry
This standard is issued under the fixed designation E2866; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This procedure covers the determination of Diisopropyl Methylphosphonate (DIMP), Ethyl Methylphosphonic Acid (EMPA),
Isopropyl Methylphosphonic Acid (IMPA), Methylphosphonic Acid (MPA)(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.
2
1.3 The Method Detection Limitmethod detection limit (MDL), electrospray ionization (ESI) mode, and Reporting Rangere-
3
porting range 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 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.
2. Referenced Documents
4
2.1 ASTM Standards:
1
This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.06 on Analytical
Methods.
Current edition approved June 1, 2016May 1, 2021. Published July 2016May 2021. Originally approved in 2012. Last previous edition approved in 20122016 as
E2866 – 12.E2866 – 12 (2016). DOI: 10.1520/E2866-12R16.10.1520/E2866-21.
2
The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B utilizing solvent extraction of soil by PFE. A detailed process
determining the MDL is explained in the reference and is beyond the scope of this Standardstandard to be explained here.
3
Reporting range concentrations are calculated from Table 4 concentrations assuming a 100 μL injection of the lowest and highest level calibration standards with a 40
mL final extract volume of a 10 gramg soil sample. Volume variations will change the reporting limit and ranges. The reporting limit (RL), lowest concentration of the
reporting range, is calculated from the concentration of the Level 1 calibration standard as shown in Table 4.
4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2866 − 21
TABLE 1 Method Detection Limit and Reporting Range
Reporting
ESI MDL
Analyte Range
Mode (PPB)
(PPB)
Diisopropyl methylphosphonate Positive 2.7 40-2000
Ethyl methylphosphonic acid Negative 2.3 40-2000
Ethyl methylphosphonic acid Positive 1.3 40-2000
Isopropyl methylphosphonic acid Negative 5.7 40-2000
Isopropyl methylphosphonic acid Positive 2.8 40-2000
Methylphosphonic acid Positive 8.7 40-2000
Pinacolyl methylphosphonic acid Negative 5.3 40-2000
TABLE 1 Method Detection Limit and Reporting Range
Reporting
ESI MDL
Analyte Range
Mode (PPB)
(PPB)
Diisopropyl methylphosphonate Positive 2.7 40–2000
Ethyl methylphosphonic acid Negative 2.3 40–2000
Ethyl methylphosphonic acid Positive 1.3 40–2000
Isopropyl methylphosphoni
...