ASTM E2787-21

Standard Test Method for Determination of Thiodiglycol in Soil Using Pressurized Fluid Extraction Followed by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

SIGNIFICANCE AND USE
5.1 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC). Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents, or have a number of other commercial uses. They are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. Schedule 2 chemicals can be found in applications unrelated to chemical weapons. TDG is both a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.5  
5.2 This method has been investigated for use with soil.
SCOPE
1.1 This procedure covers the determination of thiodiglycol (TDG) in soil using pressurized fluid extraction (PFE). A commercially available PFE system2 is used, followed by analysis using liquid chromatography (LC), and detected with tandem mass spectrometry (MS/MS). TDG is qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting range for TDG are listed in Table 1.  
1.2.1 The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B.  
1.2.2 The reporting limit (RL) is calculated from the concentration of the Level 1 calibration standard as shown in Table 4. The RL for this method is 200 ppb. Reporting range concentrations are calculated from Table 4 concentrations assuming a 5 μL injection of the lowest level calibration standard, 5 g sample, and a 2 mL final extract volume.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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: E2787 − 21
Standard Test Method for
Determination of Thiodiglycol in Soil Using Pressurized
Fluid Extraction Followed by Single Reaction Monitoring
Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/
1
MS)
This standard is issued under the fixed designation E2787; 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 mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This procedure covers the determination of thiodiglycol
(TDG) in soil using pressurized fluid extraction (PFE). A
2 2. Referenced Documents
commercially available PFE system is used, followed by
3
2.1 ASTM Standards:
analysis using liquid chromatography (LC), and detected with
tandemmassspectrometry(MS/MS).TDGisqualitativelyand D1193Specification for Reagent Water
D2777Practice for Determination of Precision and Bias of
quantitativelydeterminedbythismethod.Thismethodadheres
to single reaction monitoring (SRM) mass spectrometry. Applicable Test Methods of Committee D19 on Water
D5681Terminology for Waste and Waste Management
1.2 The method detection limit (MDL) and reporting range
E2554Practice for Estimating and Monitoring the Uncer-
for TDG are listed in Table 1.
tainty of Test Results of a Test Method Using Control
1.2.1 TheMDLisdeterminedfollowingtheCodeofFederal
Chart Techniques
Regulations, 40 CFR Part 136, Appendix B.
2.2 Other Documents:
1.2.2 The reporting limit (RL) is calculated from the con-
EPApublication SW-846Test Methods for Evaluating Solid
centrationoftheLevel1calibrationstandardasshowninTable
4
Waste, Physical/Chemical Methods
4. The RL for this method is 200 ppb. Reporting range
40 CFR Part 136, Appendix BThe Code of Federal Regu-
concentrations are calculated from Table 4 concentrations
lations
assuminga5µL injection of the lowest level calibration
standard, 5 g sample, anda2mL final extract volume.
3. Terminology
1.3 Units—The values stated in SI units are to be regarded
3.1 Definitions—For definitions of terms used in this test
asstandard.Nootherunitsofmeasurementareincludedinthis
method, refer to Terminology D5681.
standard.
3.2 Abbreviations:
1.4 This standard does not purport to address all of the
–3
3.2.1 mM—millimolar,1×10 moles/L
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.2.2 ND—non-detect
priate safety, health, and environmental practices and deter-
3.2.3 SRM—single reaction monitoring
mine the applicability of regulatory limitations prior to use.
3.2.4 MRM—multiple reaction monitoring
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
4. Summary of Test Method
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4.1 This is a performance-based method, and modifications
are allowed to improve performance.
1
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
Analytical Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2021. Published May 2021. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 2011. Last previous edition approved in 2016 as E2787–11 (2016). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/E2787-21. the ASTM website.
2 4
The PFE system that was used to develop this test method was Accelerated Available from National Technical Information Service (NTIS), U.S. Depart-
Solvent Extraction (ASE) which is a patented technique by Dionex, Sunnyvale, CA ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
94088. www.epa.gov/epawaste/hazard/testmethods/index.htm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2787 − 21
TABLE 1 Method Detection Limit and Reporting Range
system that is capable of performing at the flows, pressures,
Analyte MDL (ppb) Reporting Range (ppb) controlled temperatures, sample volumes, and requirements of
Thiodiglycol 54 200–16 000 the standard may be used.
7
7.1.2 Analytical Column —A reverse-phase analytical col-
umn with strong embedded basic ion-pairing groups
...

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: E2787 − 11 (Reapproved 2016) E2787 − 21
Standard Test Method for
Determination of Thiodiglycol in Soil Using Pressurized
Fluid Extraction Followed by Single Reaction Monitoring
Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/
1
MS)
This standard is issued under the fixed designation E2787; 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 thiodiglycol (TDG) in soil using pressurized fluid extraction (PFE). A
2
commercially available PFE system wasis used, followed by analysis using liquid chromatography (LC), and detected with
tandem mass spectrometry (MS/MS). TDG is qualitatively and quantitatively determined by this method. This method adheres to
single reaction monitoring (SRM) mass spectrometry.
1.2 The Method Detection Limitmethod detection limit (MDL) and Reporting Rangereporting range for TDG are listed in Table
1.
1.2.1 The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B.
1.2.2 The reporting limit (RL) is calculated from the concentration of the Level 1 calibration standard as shown in Table 4. The
RL for this method is 200 ppb. Reporting range concentrations are calculated from Table 4 concentrations assuming a 5 μL
injection of the lowest level calibration standard, 5 g sample, and a 2 mL final extract volume.
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
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.
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 June 2016May 2021. Originally approved in 2011. Last previous edition approved in 20112016 as
E2787 – 11.E2787 – 11 (2016). DOI: 10.1520/E2787-11R16.10.1520/E2787-21.
2
The PFE system that was used to develop this test method was Accelerated Solvent Extraction (ASE®)(ASE) which is a patented technique by Dionex, Sunnyvale, CA
94088.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2787 − 21
TABLE 1 Method Detection Limit and Reporting Range
Analyte MDL (ppb) Reporting Range (ppb)
Thiodiglycol 54 200–16 000
2. Referenced Documents
3
2.1 ASTM Standards:
D653 Terminology Relating to Soil, Rock, and Contained Fluids
D1193 Specification for Reagent Water
D3694D2777 PracticesPractice for PreparationDetermination of Sample Containers and for Preservation of Organic Constitu-
entsPrecision and Bias of Applicable Test Methods of Committee D19 on Water
D3740D5681 Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used
in Engineering Design and ConstructionTerminology for Waste and Waste Management
E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
2.2 Other Documents:
4
EPA publication SW-846,SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
40 CFR Part 136, Appendix B,B The Code of Federal Regulations
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D5681.
3.2 Abbreviations:
–3
3.2.1 mM—millimolar, 1 × 10 moles/L
3.2.2 ND—non-detect
3.2.3 SRM—single reaction monitoring
3.2.4 MRM—multiple reaction monitoring
4. Summary of Test Method
4.1 This is a performance based performance-based method, and modifications are allowed to improve performance.
4.2 For TDG analysis, samples are shipped to the lab between 0 and 6°C.6 °C.
...