ASTM D7598-16

Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 Thiodiglycol 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. Thiodiglycol is both a mustard gas precursor and degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes and some pesticides.4  
5.2 This test method has been investigated for use with reagent and surface water.
SCOPE
1.1 This procedure covers the determination of thiodiglycol (TDG) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). TDG is 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 US 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 TDG are listed in Table 1.  
1.4.1 The DVL is required to be at a concentration at least 3 times below the reporting limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratio at the DVL.  
1.4.2 The RL is the concentration of the level 1 calibration standard as shown in Table 2. The reporting limit for this test method is 100 μg/L.    
1.5 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.

General Information

• Status: Historical
• Publication Date: 31-Jan-2016
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaces: ASTM D7598-09e2 - Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry
• Effective Date: 01-Feb-2016
• Replaced By: ASTM D7598-16(2017) - Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry
• Effective Date: 15-Jun-2017

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:D7598 −16
Standard Test Method for
Determination of Thiodiglycol in Water by Single Reaction
Monitoring Liquid Chromatography/Tandem Mass
1
Spectrometry
This standard is issued under the fixed designation D7598; 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 D1193Specification for Reagent Water
D2777Practice for Determination of Precision and Bias of
1.1 This procedure covers the determination of thiodiglycol
Applicable Test Methods of Committee D19 on Water
(TDG) in surface water by direct injection using liquid
D3856Guide for Management Systems in Laboratories
chromatography (LC) and detected with tandem mass spec-
Engaged in Analysis of Water
trometry (MS/MS). TDG is qualitatively and quantitatively
D3694Practices for Preparation of Sample Containers and
determined by this test method. This test method adheres to
for Preservation of Organic Constituents
single reaction monitoring (SRM) mass spectrometry.
D5847Practice for Writing Quality Control Specifications
1.2 ThistestmethodhasbeendevelopedbyUSEPARegion
for Standard Test Methods for Water Analysis
5 Chicago Regional Laboratory (CRL).
E2554Practice for Estimating and Monitoring the Uncer-
1.3 The values stated in SI units are to be regarded as tainty of Test Results of a Test Method Using Control
Chart Techniques
standard. No other units of measurement are included in this
standard.
2.2 Other Documents:
EPApublication SW-846Test Methods for Evaluating Solid
1.4 The Detection Verification Level (DVL) and Reporting
3
Waste, Physical/Chemical Methods
Range for TDG are listed in Table 1.
1.4.1 The DVL is required to be at a concentration at least
3. Terminology
3 times below the reporting limit (RL) and have a signal/noise
ratio greater than 3:1. Fig. 1 displays the signal/noise ratio at
3.1 Definitions:
the DVL.
3.1.1 For definitions of terms used in this standard, refer to
1.4.2 The RL is the concentration of the level 1 calibration
Terminology D1129.
standard as shown in Table 2. The reporting limit for this test
3.2 Definitions of Terms Specific to This Standard:
method is 100 µg/L.
3.2.1 detection verification level, DVL)=, n—a concentra-
tion that has a signal/noise ratio greater than 3:1 and is at least
1.5 This standard does not purport to address all of the
3 times below the reporting limit (RL).
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.2.2 independent reference material, IRM, n—amaterialof
priate safety and health practices and determine the applica-
known purity and concentration obtained either from the
bility of regulatory limitations prior to use.
NationalInstituteofStandardsandTechnology(NIST)orother
reputable supplier. The IRM shall be obtained from a different
2. Referenced Documents
lot of material than is used for calibration.
2
2.1 ASTM Standards:
3.3 Acronyms:
D1129Terminology Relating to Water
3.3.1 CCC, n—Continuing Calibration Check
3.3.2 IC, n—Initial Calibration
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
3.3.3 LC, n—Liquid Chromatography
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
3.3.4 LCS/LCSD, n—Laboratory Control Sample/
Organic Substances in Water.
Current edition approved Feb. 1, 2016. Published May 2016. Originally
Laboratory Control Sample Duplicate
ɛ2
approved in 2009. Last previous edition approved in 2009 as D7598 – 09 . DOI:
10.1520/D7598-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from National Technical Information Service (NTIS), U.S. Depart-
Standards volume information, refer to the standard’s Document Summary page on ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
the ASTM website. 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 ----------------------
D7598−16
TABLE 1 Detection Verification Level and Reporting Range
sor and degradant as well as an ingredient in water-based inks,
4
Analyte DVL (µg/L) Reporting Range (µg/L) ballpoint pen inks, dyes and some pesticides.
Thiodiglycol 20 100–10 000
5.2 This test method has been investigated for use with
reagent and surface water.
6. Interferences
3.3.5 MDL, n—Method Detection Limit
6.1 Methodinterferencesmaybecausedbycontaminantsin
solvents, reagents, glassware and other apparatus producing
3.3.6 MeOH, n—Me
...

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.
´2
Designation: D7598 − 09 D7598 − 16
Standard Test Method for
Determination of Thiodiglycol in Water by Single Reaction
Monitoring Liquid Chromatography/Tandem Mass
1
Spectrometry
This standard is issued under the fixed designation D7598; 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
ε NOTE—This test method was changed editorially in February 2012.
2
ε NOTE—Added research report footnote to Section 16 editorially in June 2013.
1. Scope
1.1 This procedure covers the determination of thiodiglycol (TDG) in surface water by direct injection using liquid
chromatography (LC) and detected with tandem mass spectrometry (MS/MS). TDG is 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 US 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 TDG are listed in Table 1.
1.4.1 The DVL is required to be at a concentration at least 3 times below the reporting limit (RL) and have a signal/noise ratio
greater than 3:1. Fig. 1 displays the signal/noise ratio at the DVL.
1.4.2 The RL is the concentration of the level 1 calibration standard as shown in Table 2. The reporting limit for this test method
is 100 μg/L.
1.5 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
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
2.2 Other Documents:
3
EPA publication SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved Dec. 1, 2009Feb. 1, 2016. Published January 2010May 2016. Originally approved in 2009. Last previous edition approved in 2009 as D7598
ɛ2
– 09 . DOI: 10.1520/D7598-09E02.10.1520/D7598-16.
2
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.
3
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 ----------------------
D7598 − 16
TABLE 1 Detection Verification Level and Reporting Range
Analyte DVL (μg/L) Reporting Range (μg/L)
Thiodiglycol 20 100–10 000
3.2 Definitions:Definitions of Terms Specific to This Standard:
3.2.1 detection verification level (DVL),level, DVL)=, n—a concentration that has a signal/noise ratio greater than 3:1 and is at
least 3 times below the reporting limit (RL).
3.2.2 reporting limit (RL), independent reference material, IRM, n—the concentration of the lowest-level calibration standard
used for quantification. a material of known purity and concentration obtained either from the National Institute of Standards and
Technology (NIST) or other reputable supplier. The IRM shall be o
...