ASTM E2838-11(2016)

Standard Test Method for Determination of Thiodiglycol on Wipes by Solvent Extraction Followed by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

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 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC).6 Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents or have a number of other non-military commercial uses. Schedule 2 chemicals can also be found in applications unrelated to chemical weapons. These chemicals are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. TDG is a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.  
5.3 This method has been investigated for use on surface wipes. TDG is also a human metabolite resulting from sulfur mustard exposure but this method has not been investigated for such determinations.
SCOPE
1.1 This procedure details the determination of thiodiglycol (TDG), also known as 2,2’-thiobis-ethanol, on wipes with 3,3’-thiodipropanol (TDP) as the surrogate. This method is based upon solvent extraction of wipes by either sonication or a pressurized fluid extraction (PFE) technique as an alternative option. The extract is filtered, concentrated and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). TDG is qualitatively and quantitatively determined.  
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 Limit (MDL)2 and Reporting Range3 for TDG 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. (A) Chemical Abstract Service (CAS), A division of the American Chemical Society, 2540 Olentangy River Road, Columbus, OH, 43202, USA.

General Information

• Status: Historical
• Publication Date: 31-May-2016
• ICS: 97.080 - Cleaning appliances
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E2838 − 11 (Reapproved 2016)
Standard Test Method for
Determination of Thiodiglycol on Wipes by Solvent
Extraction Followed by Liquid Chromatography/Tandem
1
Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation E2838; 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 2. Referenced Documents
4
2.1 ASTM Standards:
1.1 This procedure details the determination of thiodiglycol
D653Terminology Relating to Soil, Rock, and Contained
(TDG), also known as 2,2’-thiobis-ethanol, on wipes with
Fluids
3,3’-thiodipropanol (TDP) as the surrogate. This method is
D1193Specification for Reagent Water
based upon solvent extraction of wipes by either sonication or
D3694Practices for Preparation of Sample Containers and
apressurizedfluidextraction(PFE)techniqueasanalternative
for Preservation of Organic Constituents
option. The extract is filtered, concentrated and analyzed by
D3740Practice for Minimum Requirements for Agencies
liquid chromatography/tandem mass spectrometry (LC/MS/
Engaged inTesting and/or Inspection of Soil and Rock as
MS). TDG is qualitatively and quantitatively determined.
Used in Engineering Design and Construction
1.2 Units—The values stated in SI units are to be regarded E2554Practice for Estimating and Monitoring the Uncer-
tainty of Test Results of a Test Method Using Control
asstandard.Nootherunitsofmeasurementareincludedinthis
Chart Techniques
standard.
2.2 Other Documents:
2
1.3 The Method Detection Limit (MDL) and Reporting
EPAPublication SW-846Test Methods for Evaluating Solid
3
Range for TDG are listed in Table 1. 5
Waste, Physical/Chemical Methods
The Code of Federal Regulations, 40 CFR Part 136,Appen-
1.4 This standard does not purport to address all of the
dix B
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety, health, and environmental practices and deter-
3.1 Abbreviations:
mine the applicability of regulatory limitations prior to use.
–3
3.1.1 mM—millimolar,1×10 moles/L
1.5 This international standard was developed in accor-
3.1.2 ND—non-detect
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 3.1.3 SRM—single reaction monitoring
Development of International Standards, Guides and Recom-
3.1.4 MRM—multiple reaction monitoring
mendations issued by the World Trade Organization Technical
3.1.5 VOA—volatile organic analysis
Barriers to Trade (TBT) Committee.
4. Summary of Test Method
4.1 For TDG wipe analysis, samples are shipped to the lab
1
This test method is under the jurisdiction ofASTM Committee D34 on Waste
between 0°C and 6°C. The samples are to be extracted,
Management and is the direct responsibility of Subcommittee D34.01.06 on
concentrated, and analyzed directly by LC/MS/MS within 7
Analytical Methods.
days of collection. The handling, storage, preservation, and
CurrenteditionapprovedJune1,2016.PublishedJuly2016.Originallyapproved
in 2011. Last previous edition approved in 2011 as E2838–11. DOI: 10.1520/ LC/MS/MS analysis are consistent between the two extraction
E2838-11R16.
2
The MDL is determined following the Code of Federal Regulations, 40 CFR
4
Part 136, Appendix B utilizing solvent extraction of wipes by sonication. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
Reporting range concentrations are calculated from Table 4 concentrations contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
assuminga10µLinjectionofthelowestandhighestlevelcalibrationstandardswith Standardsvolumeinformation,refertothestandard’sDocumentSummarypageon
a 2 mLfinal extract volume. Volume variations will change the reporting limit and the ASTM website.
5
ranges. The reporting limit (RL), lowest concentration of the reporting range, is Available from National Technical Information Service (NTIS), U.S. Depart-
calculated from the concentration of the Level 1 calibration standard as shown in ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
Table 4. 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

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E2838 − 11 (2016)
TABLE 1 Method Detection Limit and Reporting Range
6.2 All reagents and solvents shall be of pesticide residue
A
MDL Reporting Range purity or higher to minimize interference problems.
CAS
Analyte
Number (µg/wipe) (µg/wipe)
6.3 Matr
...

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: E2838 − 11 E2838 − 11 (Reapproved 2016)
Standard Test Method for
Determination of Thiodiglycol on Wipes by Solvent
Extraction Followed by Liquid Chromatography/Tandem
1
Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation E2838; 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 details the determination of thiodiglycol (TDG), also known as 2,2’-thiobis-ethanol, on wipes with
3,3’-thiodipropanol (TDP) as the surrogate. This method is based upon solvent extraction of wipes by either sonication or a
pressurized fluid extraction (PFE) technique as an alternative option. The extract is filtered, concentrated and analyzed by liquid
chromatography/tandem mass spectrometry (LC/MS/MS). TDG is qualitatively and quantitatively determined.
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 3
1.3 The Method Detection Limit (MDL) and Reporting Range for TDG 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
4
2.1 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
E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
2.2 Other Documents:
5
EPA Publication SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
The Code of Federal Regulations, 40 CFR Part 136, Appendix B
3. Terminology
3.1 Abbreviations:
-3
3.1.1 mM—millimolar, 1 × 10 moles/L
3.1.2 ND—non-detect
3.1.3 SRM—single reaction monitoring
1
This test method is under the jurisdiction of ASTM Committee E54 on Homeland Security Applications and is the direct responsibility of Subcommittee E54.03 on
Decontamination.
Current edition approved Nov. 1, 2011June 1, 2016. Published December 2011July 2016. Originally approved in 2011. Last previous edition approved in 2011 as
E2838 – 11. DOI: 10.1520/E2838-11.10.1520/E2838-11R16.
2
The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B utilizing solvent extraction of wipes by sonication.
3
Reporting range concentrations are calculated from Table 4 concentrations assuming a 10 μL injection of the lowest and highest level calibration standards with a 2 mL
final extract volume. 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.
5
Available from National Technical Information Service (NTIS), U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://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 ----------------------
E2838 − 11 (2016)
TABLE 1 Method Detection Limit and Reporting Range
A
MDL Reporting Range
CAS
Analyte
Number (μg/wipe) (μg/wipe)
Thiodiglycol 111-48-8 0.085 1-80
3,3’-Thiodipropanol 10595-09-2 Not done 1-80
(Surrogate) for surrogates
A
Chemical Abstract Service (CAS), A division of the American Chemical Society,
2540 Olentangy River Road, Columbus, OH, 43202, USA.
3.1.4 MRM—multiple reaction monitoring
3.1.5 VOA—volatile organic analysis
4. Summary of Test Method
4.1 For TDG wipe analysis, samples are shipped to the lab between 0°C and 6°C. The samples are to be extracted, concent
...